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Objective: To establish a high-performance liquid chromatography-mass spectrometry(HPLC-MS/MS) method for detecting 13 kind of free and bound phenolic acids(chlorogenic acid, protocatechuic acid, ferulic acid, p-coumaric acid, gallic acid, gentisic acid, vanillic acid, caffeic acid, syringic acid, sinapic acid, rosmarinic acid, salicylic acid, p-hydroxybenzoic acid) in fruits, and optimize the pre-treatment conditions to meet the detection requirements for phenolic acid content in various types of fruits., Methods: Free phenolic acids in fruits were extracted using methanol through ultrasonic extraction. Conjugated phenolic acids in the centrifuged residue were released by alkaline hydrolysis and extracted with ethyl acetate. The two extracts were combined, concentrated, and analyzed using HPLC-MS/MS. Separation was achieved using an Agilent ZORBAX SB-C_(18) chromatography column(3.0 mm×100 mm, 3.5 μm), and detection was performed in multiple reaction monitoring(MRM) mode., Results: All 13 standard phenolic acids achieved complete separation within 10 minutes, with linear correlation coefficients greater than 0.998 and detection limits ranging from 0.172 to 3.471 ng/mL. After optimization of the pre-treatment method, the recovery rates of the method for four types of fruits-apples, strawberries, oranges, and peaches-ranged from 80.0% to 119.4%, and the precision were lower than 7.00%(n=6). The result of testing on four categories of twelve types of fruits demonstrated significant variations in the content of phenolic acids among different fruits, and within the same category, the composition of phenolic acids did not exhibit consistency., Conclusion: The HPLC-MS/MS method exhibits high sensitivity, precision, and accuracy. It is suitable for the detection of both free and bound phenolic acids in various types of fruits.

In this study, a microelectrode array sensor based on boron and nitrogen co-doped vertical graphene (BNVG) was assembled to quantify salicylic acid (SA) in living plants. The influence of B and N contents on the electrochemical reaction kinetics and SA response signal was investigated. A microneedle sensor with three optimized BNVG microelectrodes (3.57 at.% B and 3.27 at.% N) was used to quantitatively analyze SA in the 0.5-100 μM concentration range and pH 4.0-9.0, with limits of detection of 0.14-0.18 μM. Additionally, a quantitative electrochemical model database based on the BNVG microelectrode sensor was constructed to monitor the growth of cucumbers and cauliflowers, which confirmed that the SA level and plant growth rate were positively correlated. Moreover, the SA levels in various vegetables and fruits purchased from the market were measured to demonstrate the practical application prospects for on-site inspection and evaluation., Competing Interests: Declaration of competing interest We declare that we have no financial and personal relationships with other people or organizations that can inappropriately influence our work, there is no professional or other personal interest of any nature or kind in any product, service and/or company that could be construed as influencing the position presented in, or the review of, the manuscript entitled, “Electrochemical needle sensor based on a B, N co-doped graphene microelectrode array for the on-site detection of salicylic acid in fruits and vegetables”., (Copyright © 2023. Published by Elsevier Ltd.)

Background: Indole-3-acetic acid (IAA) and salicylic acid (SA), pivotal regulators in plant growth, are integral to a variety of plant physiological activities. The ongoing and simultaneous monitoring of these hormones in vivo enhances our comprehension of their interactive and regulatory roles. Traditional detection methods, such as liquid chromatography-mass spectrometry, cannot obtain precise and immediate information on IAA and SA due to the complexity of sample processing. In contrast, the electrochemical detection method offers high sensitivity, rapid response times, and compactness, making it well-suited for in vivo or real-time detection applications., Results: A microneedle electrochemical sensor system crafted from disposable stainless steel (SS) wire was specifically designed for the real-time assessment of IAA and SA in plant in situ. This sensor system included a SS wire (100 μm diameter) coated with carbon cement and multi-walled carbon nanotubes, a plain platinum wire (100 μm diameter), and an Ag/AgCl wire (100 μm diameter). Differential pulse voltammetry and amperometry were adopted for detecting SA and IAA within the range of 0.1-20 μM, respectively. This sensor was applied to track IAA and SA fluctuations in tomato leaves during PstDC3000 infection, offering continuous data. Observations indicated an uptick in SA levels following infection, while IAA production was suppressed. The newly developed disposable SS wire-based microneedle electrochemical sensor system is economical, suitable for mass production, and inflicts minimal damage during the monitoring of SA and IAA in plant tissues., Significance: This disposable microneedle electrochemical sensor facilitates in vivo detection of IAA and SA in smaller plant tissues and allows for long-time monitoring of their concentrations, which not only propels research into the regulatory and interaction mechanisms of IAA and SA but also furnishes essential tools for advancing precision agriculture., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024. Published by Elsevier B.V.)

Considerable effort has been invested in developing salicylic acid (SA) biosensors for various application purposes. Here, by engineering the sensing modules and host cell chassis, we have gradually optimized the NahR-Psal/Pr-based SA biosensor, increasing the sensitivity and maximum output by 17.2-fold and 9.4-fold, respectively, and improving the detection limit by 800-fold, from 80 μM to 0.1 μM. A portable SA sensing device was constructed by embedding a gelatin-based hydrogel containing an optimized biosensor into the perforations of tape adhered to glass slide, which allowed good determination of SA in the range of 0.1 μM-10 μM. Then, we developed a customized smartphone App to measure the fluorescence intensity of each perforation and automatically calculate the corresponding SA concentration so that we could detect SA concentrations in real cosmetic samples. We anticipate that this smartphone-based imaging biosensor, with its compact size, higher sensitivity, cost-effectiveness, and easy data transfer, will be useful for long-term monitoring of SA., Competing Interests: Declaration of competing interest The authors declare no completing financial interest, and have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Chia seeds (CS) and sprouts are rich sources of phenolic compounds and polyunsaturated fatty acids (PUFA). We hypothesized that the application of chemical stressors, such as salicylic acid (SA) and hydrogen peroxide (H 2 O 2 ), would induce changes in the polyphenol and fatty acid profile of chia sprouts, leading to an increase in their nutraceutical potential. This study aimed to assess the effect of non-elicited (NE) and chemically elicited (CE with 1-mM SA and 20-mM H 2 O 2 ) sprouting on the polyphenol and fatty acid (FA) profiles of chia through high-resolution liquid chromatography-mass spectrometry and chemometric analyses. NE and CE chia sprouts showed increased content and diversity of polyphenols compared to the CS but with lower content of FA. Interestingly, rosmarinic acid was the major polyphenol identified in CS and was increased about 4-fold in all chia sprouts, whereas the major PUFA of CS, α-linolenic acid, was reduced by 39%. Regarding the chemical elicitation, the multivariate analyses indicated that SA-elicited chia sprouts were characterized by their high content of most polyphenols, mainly flavones and isoflavones, as well as a high antioxidant capacity, whereas H 2 O 2 -elicited chia sprouts were differentiated by protects their PUFA composition and seedling growth parameters. These results demonstrate that the chemical elicitation with SA and H 2 O 2 represents a promising approach for improving sprouts' nutraceutical quality and could be used in further research to develop strategies for agriculture and food production., (© 2024. The Author(s), under exclusive licence to Springer Science+Business Media, LLC, part of Springer Nature.)

Willow (Salix spp.) is gaining an increasing interest as a fast-growing tree with high biomass yield from low agricultural inputs, which contains potentially bioactive compounds. The present work aimed to develop a high-yield extraction procedure combined with robust, sensitive and fast microLiquid Chromatography-Triple Quadrupole Mass Spectrometry (LC-MS/MS) based method for comprehensively quantifying flavonoids and salicylic acid in the bark of Salix spp. We have investigated the effect of freeze- and oven-drying procedures and five extraction solvents on the yield of individual flavonoid and salicylic acid when performing classical solid-liquid extraction. The freeze-drying was the best drying procedure for preserving monomeric and polymeric flavan-3-ols, whereas other flavonoids were less affected. Salicylic acid was not affected by the drying procedures. The best extraction solvent in terms of the yield of individual flavonoid among the tested solvents in this study was the combination of methanol acidified with 1% hydrochloric acid. LC-MS/MS method has shown a high recovery percentage (≥80%), good precision and overall robustness., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 The Authors. Published by Elsevier B.V. All rights reserved.)

Salicylic acid (SA) is a key hormone that regulates plant growth and immunity, and understanding the physiologic processes induced by SA enables the development of highly pathogen-resistant crops. Here, we report the synthesis of three new SA-sensors (R1-R3) from hydroxyphenol derivatives of a rhodamine-acylhydrazone scaffold and their characterization by NMR and HRMS. Spectroscopic analyses revealed that structural variations in R1-R3 resulted in sensors with different sensitivities for SA. Sensor R2 (with the 3-hydroxyphenyl modification) outperformed R1 (2-hydroxyphenyl) and R3 (4-hydroxyphenyl). The SA-detection limit of R2 is 0.9 μM with an ultra-fast response time (<60 s). In addition, their plant imaging indicated that designed sensor R2 is useful for the further study of SA biology and the discovery and development of new inducers of plant immunity.

Banana harvesting generates a large amount of banana pseudostem waste, which is generally burnt or thrown away, despite containing many nutrients. Bio-enriched organic fertilizer (BOF) was prepared from banana pseudostem sap (BPS), and it has been patented (Patent No. WO 2013/001478 Al). Several reports revealed that its application increases plant growth promotion of various horticulture crops. Apart from macro- and micronutrients, it also contained phytohormones. Hence, the present study aims to detect and quantify phytohormone in it. A novel method was developed to extract four phytohormones, viz., indole-3-acetic acid (IAA), indole-3-butyric acid (IBA), gibberellic acid (GA 3 ), and salicylic acid (SA) using single solvent from BPS and BOF. Extracted hormones were analyzed by ultrahigh-performance liquid chromatography coupled with heated electrospray ionization tandem mass spectrometry (UHPLC-HESI-MS/MS). BOF showed a higher concentration of IAA, IBA, GA 3 , and SA than BPS. Thus, this is the first time a method has been reported to extract and detect phytohormones from banana pseudostem sap., (© 2022. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.)

Anthracene biodegradation potential has been studied in liquid culture and soil microcosm environment by employing green synthesized TiO 2 nanoparticles (NPs) and Alcaligenes faecalis HP8. The bacterium was isolated from crude oil contaminated soil, while TiO 2 nanoparticles were synthesized using Paenibacillus sp. HD1PAH and Cyperus brevifolius which have PAHs remediation abilities. The dual application of TiO 2 nanoparticles and Alcaligenes faecalis HP8 decreases anthracene concentration up to 21.3% in liquid at the end of 7 days and 37.9% in the soil treatments after completion of 30 days. Besides, the GC-MS analysis revealed production of five metabolites including 1,2-anthracenedihydrodiol; 6,7-benzocoumarin; 3-hydroxy-2-naphthoic acid; salicylic acid and 9,10-anthraquinone at different time interval of the treatments. Anthracene degradation pathway confirms the breakdown of three ring anthracene to one ring salicylic acid. Additionally, soil dehydrogenase, urease, alkaline phosphatase, catalase and amylase activities increased up to 4.09 folds, 8.6 folds, 4.4 folds, 3.6 folds and 2.1 folds respectively after the combined treatments of TiO 2 nanoparticles and Alcaligenes faecalis HP8. The bacterial biomass and residual anthracene concentration were found to be negatively correlated. Finally, the study brings into light a novel anthracene biodegradation pathway and provides a new dimension in nano assisted bacterial remediation., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier Ltd. All rights reserved.)

This study describes the development of a fully manual method for on-site dispersive liquid-liquid microextraction based on the direct solidification of switchable-hydrophilicity salicylic acid (on-site DLLME-DSSA) coupled with high-performance liquid chromatography with an ultraviolet detector (HPLC-UVD) and its utilization for the detection of benzoylurea insecticides (BUs) in water and honey samples. Salicylic acid (SA), a switchable hydrophilic aromatic acid, was used as an extraction solvent. It can be converted into the hydrophobic/hydrophilic forms in pH-changeable solutions, facilitating facile and effective dispersion and phase separation. Moreover, the melting point of SA (significantly higher than room temperature) enables its direct solidification without an ice-water bath, facilitating its collection by filtration. The dispersion, separation, and collection of the extraction solvent were carried out entirely in a plastic syringe without requiring special apparatus or additional energy. Univariate and response surface analyses were used to optimize various parameters of the on-site DLLME-DSSA method. Under optimal conditions, the limits of determination (LODs) were 1.50 µg L -1 and 0.03-0.09 mg kg -1 in water and honey, respectively. The relative standard deviations (RSDs) for inter-day (n = 5) and intra-day (n = 5) precision were ≤8.4%, whereas the extraction recoveries and enrichment factors for the BUs ranged from 67.0 to 97.1% and 29 to 34, respectively. Furthermore, the proposed method was used for the on-site extraction and laboratory detection of BUs from real water and honey samples. Theoretical analyses indicated non-covalent interactions (such as hydrogen bonds, electrostatic interactions, van der Waals forces, and π-π interactions) to be the main driving force for extraction. This study introduces a switchable hydrophilic aromatic acid capable of direct solidification into on-site DLLME for the first time, opening new frontiers in the development of on-site sample pretreatment methods., Competing Interests: Declaration of Competing Interest The authors have declared that there are no conflicts of interest., (Copyright © 2022. Published by Elsevier B.V.)

This experiment was conducted in the poultry field of the College of Agriculture, University of Diyala, and the Biochemistry Laboratory in the Department of Animal Production to show the effect of using tartaric and salicylic acids on the chemical composition of eggs produced by Lohman chickens raised at high temperatures, in which 210 laying hens of brown Lohman strain were used. Sixty weeks were divided into seven treatments: T1, the control treatment, T2 and T3, in which 0.2% of tartaric and salicylic acid were added to drinking water, respectively, and T4 added to it a mixture of organic acids at a rate of 0.4% to the drinking water, and treatments T5 and T6 were added. It contained 0.2% of tartaric and salicylic acid to the ration, respectively, and T7 was added to the ration of 0.4% of the two organic acids to the diet formulation. At the age of 75 weeks, eggs were taken randomly from the treatments and at a rate of 5 eggs/treatment to know the effect of the treatments on the chemical composition of the eggs produced, and the results of the statistical analysis showed It is proved in Appendix 1 that there was no significant effect ( P ≥0.05) of the different treatments on the studied traits, which included the percentage of moisture, protein, fat, carbohydrates and ash in each of the whites and yolks. The present study showed that adding tartaric and salicylic acids to water and feed did not significantly affect the quality of eggs produced from Lohman chickens., Competing Interests: The authors declare that they have no conflict of interest.

The widespread distribution of contaminants of emerging concern (CECs) is a major concern due to their potential effects on human health and the environment. The insufficient sewage treatment plant infrastructures is a global problem most accentuated in less developed countries and results in the discharge of CECs to water bodies. Pacu (Piaractus mesopotamicus) is a ray-finned freshwater fish species native to the Paraná basin. It is also the most produced aquaculture fish species in Argentina since 2012. Though uninvestigated to date, the occurrence of CECs in pacu may be of high relevance due to production volumes and relevance to human exposure through fish consumption. In this study, we applied a high-resolution mass spectrometry screening method to qualitatively analyze over 100 CECs in pacu. Four extraction/cleanup methods were tested on pooled pacu fillet, including solid-phase extraction and QuEChERS. The method that produced the highest number of detections was selected for further analysis of pacu purchased in supermarkets and fish markets in Argentina between 2017 and 2020. Residues of pesticides, antibiotics, pharmaceuticals, personal care products, plasticizers, sweeteners, drug metabolites, stimulants, and illegal drugs were detected in the samples. A total of 38 CECs were detected, ranging between 24 and 35 CECs per individual sample. 100% of the samples had positive detections of caffeine, 1,7-dimethylxanthine, xanthine, benzoylecgonine, methylparaben, ethylparaben, bis(2-ethylhexyl) phthalate (DEHP), metolachlor, carbendazim, salicylic acid, 2,4-D, saccharin, cyclamate, and dodecanedioic acid. Mappings generated with correspondence analysis were used to explore similarities/dissimilarities among the detected compounds. To our knowledge this is the first report of saccharin, cyclamate, 2,4 - D, carbendazim, metolachlor, ethylparaben, propylparben, bisphenol A, DEHP, and benzotriazole in fish from Argentina, and the first report on the presence of lisinopril, metropolol acid and dodecanedioic acid in fish worldwide., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

Aspirin is a widely used anti-inflammatory drug. It is reported that a relationship may exist between salicylic acid content in plasma and saliva after taking aspirin. This study established a rapid, convenient, and safe method to assess salicylic acid concentration in human saliva. A novel HPLC-ultraviolet detector was used to measure salicylic acid concentrations in human saliva and plasma. A C18 reversed-phase column with an aqueous solution of 0.1% trifluoroacetic acid (TFA)-acetonitrile mobile phase was used, and drug peaks were recorded at 303 nm. Salicylic acid was completely separated in saliva and plasma. Excellent linearity and correlation (r 2 ≥ 0.9999) was observed between 0.1 and 2.0 μg/mL. The detection limit (S/N = 3) was 33 ng/mL, and intra- and inter-day recoveries were 103.5-113.3% and 101.1-109.5%, respectively. Salicylic acid was measured within nine hours after administration of acetylsalicylic acid tablets. A positive correlation between salicylic acid content in saliva and plasma was found (r = 0.867, p < 0.001). The proposed method was used successfully to measure salicylic acid concentration in human saliva. Meanwhile, we explored the relationship between salicylic acid levels in plasma and saliva. Saliva might replace blood for monitoring aspirin treatment. In addition, the research provides a reference for application to saliva samples., (Copyright © 2022 Elsevier B.V. All rights reserved.)

Background: Oral anti-platelet agents are the cornerstone of the treatment of multiple cardiovascular diseases and in the long-term prevention of their recurrence., Objective: In the present work, we report a method based on micellar liquid chromatography coupled with ultraviolet detection (MLC/UV), for the simultaneous quantification of combined anti-platelet therapy namely, clopidogrel bisulfate (CPS), aspirin (ASP), together with salicylic acid (SA), in their pharmaceutical dosage form., Methods: The incorporation of 0.1M polyoxyethylene 23 lauryl ether (Brij-35) as a surfactant into the mobile phase improved solute-mobile phase interaction allowing for minimal organic solvent utilization, enhanced resolution, and rapid analysis (7 min). Furthermore, we performed a comprehensive evaluation of the environmental impact caused by our procedures versus previously reported analytical procedures applied in the determination of CPS and ASP. The evaluation was made using the Eco-scale tool., Results: The results of the developed method indicated the superiority of our procedures in terms of greenness without compromising the quality of performance characteristics. The method was linear in the range of 1-100 µg/mL with limits of detection of 0.28, 0.32, and 0.29 µg/mL for CPS, ASP, and SA, respectively. The developed method can also be utilized to test the purity and the stability of ASP in pharmaceutical formulations through monitoring SA as its main degradation product., Conclusion: The MLC/UV method was successfully applied to the quantitative analysis of CPS, ASP together with SA-as a main degradation product of ASP-in their pharmaceutical dosage form., Highlights: The developed method was successfully applied for the determination of clopidogrel bisulfate (CPS), aspirin (ASP), together with salicylic acid (SA), in their pharmaceutical dosage form., (© The Author(s) 2022. Published by Oxford University Press on behalf of AOAC INTERNATIONAL. All rights reserved. For permissions, please email: journals.permissions@oup.com.)

Background: The application of kaolin particle film is considered a short-term strategy against several environmental stresses in areas with a Mediterranean-like climate. However, it is known that temperature fluctuations and water availability over the season can jeopardize kaolin efficiency in many Mediterranean crops. Hence, this study aims to evaluate the effects of kaolin foliar application on berry phytohormones, antioxidant defence, and oenological parameters at veraison and harvest stages of Touriga-Franca (TF) and Touriga-Nacional (TN) grapevines in two growing seasons (2017 and 2018). The 2017 growing season was considered the driest (-147.1 dryness index) and the warmest (2705 °C growing degree days) of the study., Results: In 2017, TF kaolin-treated berries showed lower salicylic acid (-26.6% compared with unsprayed vines) and abscisic acid (ABA) (-10.5%) accumulation at veraison, whereas salicylic acid increased up to 28.8% at harvest. In a less hot season, TN and TF kaolin-treated grapevines showed a twofold in ABA content and a threefold increase in the indole-3-acetic acid content at veraison and lower ABA levels (83.8%) compared with unsprayed vines at harvest. Treated berries showed a decreased sugar content, without compromising malic and tartaric acid levels, and reactive oxygen species accumulation throughout berry ripening., Conclusion: The results suggest kaolin exerts a delaying effect in triggering ripening-related processes under severe summer stress conditions. Treated berries responded with improved antioxidant defence and phytohormone balance, showing significant interactions between kaolin treatment, variety, and developmental stage in both assessed years. © 2021 Society of Chemical Industry., (© 2021 Society of Chemical Industry.)

Measuring quantitative changes in plant hormones and derivatives is crucial to understand how reactive oxygen species trigger signaling cascades to regulate stress responses. In this chapter, we describe the liquid chromatography-mass spectrometry procedure that we use to extract and quantify salicylic acid (SA), jasmonic acid (JA), and related compounds in common extracts of Arabidopsis tissue. The method can provide quantitative data on SA, SA glucosides, and JA, as well as information on oxidized and conjugated forms of these compounds and related derivatives of benzoic acid., (© 2022. Springer Science+Business Media, LLC, part of Springer Nature.)

Transcriptional factor-based biosensors (TFBs) have been widely used in dynamic pathway control or high-throughput screening. Here, we systematically explored the tunability of a salicylic acid responsive regulator MarR from Escherichia coli aiming to explore its engineering potential. The effect of endogenous MarR in E. coli on the MarR-PmarO biosensor system was investigated. Furthermore, to investigate the function of marO binding boxes in this biosensor system, a series of hybrid promoters were constructed by placing the marO binding boxes in the strong constitutive pL promoter. The engineered hybrid promoters became responsive to MarR and salicylic acid. To further study the influence of each nucleotide in the marO box on MarR binding, we employed dynamic modeling to simulate the interaction and binding energy between each nucleotide in the marO boxes with the corresponding residues on MarR. Guided by the results of the simulation, we introduced mutations to key positions on the hybrid promoters and investigated corresponding dynamic performance. Two promoter variants I12AII4T and I12AII14T that exhibited improved responsive strengths and shifted dynamic ranges were obtained, which can be beneficial for future metabolic engineering research.

At present, screening of active ingredients from natural products for pharmacological and clinical research is mostly time-consuming and costly. In this study, a molecular network (MN) guided high performance liquid chromatography-ultraviolet-fluorescence detector (HPLC-UV-FLD) method was carried out to profile the global antioxidant activity compounds, including the trace amount ingredients in Camellia nitidissima Chi (CNC). Firstly, HPLC-UV-FLD postcolumn derivatization system was utilized to screen the antioxidants. Then the MN of CNC was established via mass spectrometry (MS) data for getting the connection between ingredient structures. As a result, HPLC-UV-FLD indicated three antioxidant ingredients: gallic acid (126.3 mg/g), catechin (564.8 mg/g), and salicylic acid (24.3 mg/g). Combined with the MN, the actives' precise location and connection relationship were clarified based on the structural similarities. A new antioxidant ingredient, okicamelliaside, was suggested and evaluated at free radical scavenging and enzymatic protection. The novel method of activity and structural correlation analysis based on MN could provide a useful guide for screening trace active ingredients in natural products. PRACTICAL APPLICATION: Three main ingredients were screened out from Camellia nitidissima Chi by HPLC-UV-FLD postcolumn derivatization system. Integrated molecular network and HPLC-UV-FLD analysis, a new type of antioxidant okicamelliaside was selected. The novel method of activity and structural correlation analysis based on molecular network could provide a useful guide for screening trace active ingredients in natural products., (© 2021 Institute of Food Technologists®.)

Fusarium verticillioides causes multiple diseases of Zea mays (maize) including ear and seedling rots, contaminates seeds and seed products worldwide with toxic chemicals called fumonisins. The role of fumonisins in disease is unclear because, although they are not required for ear rot, they are required for seedling diseases. Disease symptoms may be due to the ability of fumonisins to inhibit ceramide synthase activity, the expected cause of lipids (fatty acids, oxylipins, and sphingolipids) alteration in infected plants. In this study, we explored the impact of fumonisins on fatty acid, oxylipin, and sphingolipid levels in planta and how these changes affect F. verticillioides growth in maize. The identity and levels of principal fatty acids, oxylipins, and over 50 sphingolipids were evaluated by chromatography followed by mass spectrometry in maize infected with an F. verticillioides fumonisin-producing wild-type strain and a fumonisin-deficient mutant, after different periods of growth. Plant hormones associated with defense responses, i.e., salicylic and jasmonic acid, were also evaluated. We suggest that fumonisins produced by F. verticillioides alter maize lipid metabolism, which help switch fungal growth from a relatively harmless endophyte to a destructive necrotroph.

Two green, simple, and accurate chromatographic methods were developed and validated for the simultaneous determination of omeprazole and aspirin mixture in the presence of salicylic acid, a major impurity of aspirin. Method A is a reversed-phase ultra-high-performance liquid chromatography; the separation was performed on a C18 column, with a mobile phase composed of ethanol:0.1% aqueous solution of triethylamine acidified with orthophosphoric acid (pH 3) (30:70, v/v) at 0.15 mL/min flow rate and 230 nm. Omeprazole, aspirin, and aspirin impurity retention times were 7.47, 4.40, and 5.13 min, respectively. Good linearity was achieved in the concentration ranges of 5-80, 5-85, and 3-50 μg/mL for the three mentioned components, respectively. Method B is thin-layer chromatography (TLC) where silica gel TLC F254 plates were utilized to achieve separation using ethanol:ethyl acetate (2:8, v/v) as a developing system at 240 nm. The resulted R f values were 0.83, 0.65, and 0.23 for omeprazole, aspirin, and impurity, respectively. The concentration ranges of 0.1-3 μg/band for the three drugs showed good linearity. The proposed methods are eco-friendly and greener when compared to the already reported method (Microchemical Journal, 152, 104350). This is the first use of TLC method for the determination of the three drugs. International Council for Harmonization (ICH) guidelines were followed to ensure the validity of developed methods., (© 2020 John Wiley & Sons, Ltd.)

While many studies have been conducted on drug-inducing alterations in the aquatic environment, little is known about their interaction with climate change, such as rising temperatures. To increase knowledge on this topic, Mytilus galloprovincialis mussels were exposed to two different temperatures 17 ± 1 °C (control) and 21 ± 1 °C in the absence and presence of salicylic acid (SA) (4 mg/L) for 28 days. Salicylic acid in the water and tissues was measured and its impact reported through biomarker responses including: energy metabolism (electron transport system (ETS) activity, glycogen (GLY), protein (PROT) and lipids (LIP) contents), oxidative stress markers (activity of the enzymes superoxide dismutase (SOD), catalase (CAT), and glutathione peroxidase (GPx)), glutathione balance between the reduced and the oxidized forms (GSH/GSSG), and damage to membrane lipids (lipid peroxidation - LPO). The mussels responded differently if the stresses imposed were single or combined, with greater impacts when both stressors were acting together. Contaminated mussels exposed to high temperatures were unable to increase their metabolic capacity to restore their defence mechanisms, reducing the expenditure of LIP. In the presence of SA and increased temperature antioxidant defences respond differently, with higher SOD levels and inhibition of CAT. The present study highlights not only the negative impact of warming and SA, but especially how temperature increase will promote the impact of SA in M. galloprovincialis, which under predicted climate change scenarios may greatly impair population maintenance and ecosystem biodiversity., (Copyright © 2020 Elsevier B.V. All rights reserved.)

Some recent results reported that aspirin (acetylsalicylic acid) had a positive effect on the treatment of certain types of cancer. However, the results cannot be generalized and it is not always clear whether it is a direct anticancer effect or a general health effect. Since plants produce different amounts of salicylic acid, we have sought a relationship between the salicylic acid content of some plant extracts and their anticancer activity. Growing of wheat and rice plants were carried out under controlled conditions. The salicylic acid content was determined by high-performance liquid chromatography. The viability and cell cycle assays were performed on HepG2 and Caco-2 cell lines. Despite the high content of salicylic acid, the extracts from rice plants did not show significant anticancer activity. In spite of the low salicylic acid content, the positive effect of wheat germ was confirmed in both tests. There is no direct relationship between the salicylic acid content of the plant extracts and their anticancer activity. However, it has been proven that young wheat germ is more effective than mature leaf., (© 2020. The Author(s).)

Agronomically important traits often develop during the later stages of crop growth as consequences of various plant-environment interactions. Therefore, the temporal physiological states that change and accumulate during the crop's life course can significantly affect the eventual phenotypic differences in agronomic traits among crop varieties. Thus, to improve productivity, it is important to elucidate the associations between temporal physiological responses during the growth of different crop varieties and their agronomic traits. However, data representing the dynamics and diversity of physiological states in plants grown under field conditions are sparse. In this study, we quantified the endogenous levels of five phytohormones - auxin, cytokinins (CKs), ABA, jasmonate and salicylic acid - in the leaves of eight diverse barley (Hordeum vulgare) accessions grown under field conditions sampled weekly over their life course to assess the ongoing fluctuations in hormone levels in the different accessions under field growth conditions. Notably, we observed enormous changes over time in the development-related plant hormones, such as auxin and CKs. Using 3' RNA-seq-based transcriptome data from the same samples, we investigated the expression of barley genes orthologous to known hormone-related genes of Arabidopsis throughout the life course. These data illustrated the dynamics and diversity of the physiological states of these field-grown barley accessions. Together, our findings provide new insights into plant-environment interactions, highlighting that there is cultivar diversity in physiological responses during growth under field conditions., (© The Author(s) 2020. Published by Oxford University Press on behalf of Japanese Society of Plant Physiologists. All rights reserved. For permissions, please email: journals.permissions@oup.com.)

Plants have excellent abilities to regenerate from detached tissues, in which various phytohormones play critical roles. It has been reported that jasmonate and auxin appeared sequentially during direct de novo root regeneration (DNRR) after leave detachment. However, the role of salicylic acid (SA) is still unknown in this procedure although it is another important plant hormone. We have demonstrated the potential of electrochemical sensors for real time screening of SA but the stability still needed to be improved. Herein a digital plotter was used to modify the carbon tape modified electrodes with pencil traces in order to improve the reproducibility. The modified electrodes in paper-based analytical devices were applied to monitor SA during direct DNRR. The drawing routines and the distances between two close traces were optimized. Our results showed that the carbon tape modified electrodes achieved more reproducible responses of SA. Combined with in vivo sampling, the results using our approach demonstrated that amounts of SA in the wild Arabidopsis thaliana leaves during direct DNRR reached highest at around 72 h after detachment and then decreased, implying that the wave of SA contents might follow that of auxin during direct DNRR. The application of the digital plotter offered a cost-effective and more reproducible method for preparation of disposable working electrodes, which might be extended for other biochemical assays., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier B.V. All rights reserved.)

Salicylates are among the most known anti-inflammatory drugs, used both in human and veterinary medicine. They also occur naturally in plants. Residues of salicylic acid in tissues and eggs may occur after drug administration or exposure of animals to feed material with high salicylate content. An animal study was performed on laying hens. The birds received sodium salicylate or acetylsalicylic acid (10 mg/kg b.w.) for 7 days or were given corn containing 1.18 mg/kg of salicylic acid. Samples of liver, muscle and plasma were collected at 0, 4, 8, 24 and 72 h after treatment; eggs were collected daily for 14 days. Salicylic acid and its metabolites: gentisic acid, salicyluric acid and gentisuric acid were determined using liquid chromatography coupled with tandem mass spectrometry. In both liver and muscle, the residues after administration of sodium salicylate were initially higher than for acetylsalicylic acid but they depleted at the same time. The deposition and depletion profile of salicylic acid in eggs was similar for groups receiving both drugs; the plateau level reached 248 ± 61.5 μg/kg and 275 ± 82.1 μg/kg. The concentration of salicylic acid in tissues and eggs of animals receiving salicylic acid was low. Gentisic acid was found in individual samples of liver, muscle and eggs from all treated groups. The exposure of hens to the salicylates at feed additive levels and to naturally occurring salicylates results in low residue concentrations and fast depletion of salicylic acid. The eggs do not pose any risk to consumers sensitive to salicylates.

In the context of future climate change new habitats will be threatened and unique species will be forced to develop different strategies to survive. Saxifraga longifolia Lapeyr. is an endemic species from the Pyrenees with a very particular habitat. We explored the capacity and strategies of S. longifolia plants to face different severities of drought stress under both natural conditions and controlled water stress followed by a re-watering period of 20 days. Our results showed a role for abscisic acid (ABA), salicylic acid (SA) and cytokinins (CKs) in plant survival from drought stress, and as the stress increased, ABA lost significance and SA appeared to be more associated with the response mechanisms. Moreover, photo-oxidative stress markers revealed that both xanthophyll cycles played a photoprotection role with a stronger participation of the lutein epoxide cycle as the stress was more intense. Severe drought decreased the maximum efficiency of photosystem II (F v /F m ) below 0.45, being this the limit to survive upon rewatering. Overall, our results proved different strategies of S. longifolia plants to cope with drought stress and suggested a F v /F m threshold to predict plant survival in high-mountain environments., (© 2020 Scandinavian Plant Physiology Society.)

Phytohormones and reactive oxygen species mediate processes such as germination and dormancy. The elucidation of the physiological and biochemical events implicated in the transition from dormancy to germination in different plant species such as sunflower becomes a topic of interest. In this study, we investigated the spatiotemporal variation of salicylic acid (SA), hydrogen peroxide (H 2 O 2 ) and the activity of two antioxidant enzymes (catalase, CAT - EC 1.11.1.6 and ascorbate peroxidase - EC 1.11.1.11) in embryonic axis and cotyledons of dry and imbibed seeds of dormant (B123) and non-dormant (B91) sunflower lines. The results showed that embryonic axis had higher level of SA and H 2 O 2 than cotyledons in both lines. In dry seeds, B123 embryo (embryonic axis + cotyledons) showed a higher SA content than B91. After dry storage at room temperature, SA decreased in B123 embryos to a value close to that registered in B91 embryos. B123 embryonic axis of dry seeds presented higher H 2 O 2 levels than B91. Dry storage led to an increase of H 2 O 2 levels and a decrease of CAT activity in B123 embryonic axis. During imbibition, B123 seeds stored for 33 days displayed an increase in SA level in the embryonic axis (3 h of imbibition) and this lower level correlated with a decrease in H 2 O 2 (6 h of imbibition). Thus, the embryo-imposed dormancy in B123 dry seeds was associated with high levels of SA and low H 2 O 2 , whereas the dormancy release was linked with SA decrease and increase of H 2 O 2 as a consequence of lower CAT activity., (© 2019 Scandinavian Plant Physiology Society.)

Detecting plant-derived signal molecules using fluorescent probes is a key topic and a huge challenge for scientists. Salicylic acid (SA), a vital plant-derived defense hormone, can activate global transcriptional reprogramming to systemically express a network of prominent pathogenesis-related proteins against invasive microorganisms. This strategy is called systemic acquired resistance (SAR). Therefore, monitoring the dynamic fluctuations of SA in subcellular microenvironments can advance our understanding of different physiological and pathological functions during the SA-induced SAR mechanism, thus benefiting the discovery and development of novel immune activators that contribute to crop protection. Here, detection of signaling molecule SA in plant callus tissues was first reported and conducted by a simple non-fluorescent rhodamine-tagged architecture bearing a flexible 2-amino- N , N -dimethylacetamide pattern. This study can markedly advance and promote the usage of fluorescent SA probes for distinguishing SA in the plant kingdom.

Salicylic acid (SA) is a key natural component that mediates local and systemic resistance to pathogens in many dicotyledonous species. However, its function is controversial in disease resistance in rice plants. Here, we show that the SA signaling is involved in both pathogen-associated-molecular-patterns triggered immunity (PTI) and effector triggered immunity (ETI) to Xanthomonas oryzae pv. Oryzae (Xoo) mediated by the recessive gene xa5, in which OsNPR3.3 plays an important role through interacting with TGAL11. Rice plants containing homozygous xa5 gene respond positively to exogenous SA, and their endogenous SA levels are also especially induced upon infection by the Xoo strain, PXO86. Depletion of endogenous SA can significantly attenuate plant resistance to PXO86, even to 86∆HrpXG (mutant PXO86 with a damaged type III secretion system). These results indicated that SA plays an important role in disease resistance in rice plants, which can be clouded by high levels of endogenous SA and the use of particular rice varieties.

Salicylic acid is an emerging environmental contaminant, usually found at ng/L concentrations in natural waters. Its quantification usually involves liquid chromatography-tandem mass spectrometry, which requires complex and costly instrumentation as well as time-consuming sample pretreatment, typically involving large solvent volumes. In this work, sequential injection chromatography was exploited to develop a fast, green, cost-effective, and highly sensitive procedure for fluorimetric determination of salicylic acid in natural waters. Analyte preconcentration directly on the chromatographic column (on-column preconcentration) was exploited to improve detectability, yielding an enrichment factor of 122 (1.75 mL of sample) and takes only 8.5 min per determination. A detection limit of 20 ng/L, a linear response range from 0.06 to 5.00 µg/L, coefficients of variation lower than 3.0% (n = 10), and recoveries within 86 and 114% were estimated. The procedure was applied for the analyses of freshwater samples and results agreed with those obtained by liquid chromatography-tandem mass spectrometry at the 95% confidence level. The proposed procedure encompasses in-line concentration, isolation/separation, and detection, without the need for sample clean-up, thus minimizing the consumption of organic solvents and risk of analyte losse., (© 2020 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

The determination of salicylic acid (SA), an important phytohormone responsible for stress signaling in plants, is of great importance in agricultural studies. However, a critical evaluation of the procedures for the extraction of the analytes and hydrolysis of the conjugated forms of SA is lacking in the literature and the available alternatives are complex, time-consuming, and laborious. In this study, the sample preparation methods for SA fractionation were critically evaluated to develop a simpler and faster alternative procedure. Microwave-assisted extractions were carried out with 2.0 g of fresh leaves and 8.0 mL of a 75% v/v ethanol:water solution at 40 °C for 10 min, followed by alkaline hydrolysis using 100 μL of 0.1 mol L -1 NaOH at 80 °C for 60 min. Free and total SA were determined in crude and hydrolyzed extracts, respectively, by fluorimetry after chromatographic separation of the sample matrix under isocratic elution (25% v/v acetonitrile/phosphate buffer) using a C18 column. Recovery experiments using methyl salicylate and acetylsalicylic acid model compounds demonstrated that the soft microwave-assisted extraction did not decompose the SA derivatives and that alkaline hydrolysis was quantitative. The proposed procedure was successfully applied for fractionation of SA in sugarcane, corn, and soybean leaves with extraction and hydrolysis yields up to 70 and 20% higher than those achieved in previously proposed approaches, respectively. The developed procedure is a simple, fast, and reliable alternative for SA fractionation in crude extracts without sample clean-up, and utilizes dilute reagents and green solvents., (Copyright © 2019 Elsevier B.V. All rights reserved.)

A bstract: Litsea cubeba (Lour.) Pers., a popular essential oil plant, is a dioecious species with degenerative sexual organs in both male and female individuals. Yet, the mechanism of degenerative organs development in male and female flowers is poorly understood. Here, we analyzed the morphological characters of degenerative organ development by morphological and histological observations, and determined the critical stage of abortion that occurs at pre-meiosis in male and female flowers. We also conducted RNA sequencing (RNA-seq) to understand the genetic basis of stamen abortion in female flowers. The differentially expressed genes (DEGs) were identified during the staminode development in female flowers; functional enrichment analysis revealed some important biological pathways involved the regulation of stamen abortion, including plant hormone signal transduction, phenylpropanoid biosynthesis, flavonoid biosynthesis and monoterpenoid biosynthesis. Furthermore, 15 DEGs involved in the hormone pathways were found to regulate stamen development. By HPLC-MS/MS analysis, there were a salicylic acid (SA) content peak and the gibberellin (GA) content lowest point in the abortion processes in female flowers, suggesting a vital function of hormonal processes. Co-expression network analysis further identified several hub genes that potentially played significant roles in the stamen abortion of L. cubeba . Taken together, we proposed a model involved in plant hormones pathways underlying stamen abortion during pre-meiosis in female flowers of L. cubeba ., Competing Interests: The authors declare no conflicts of interest.

Heavy metals such as cadmium and zinc constitute major pollutants in coastal areas and frequently accumulate in salt marshes. The wetland halophyte plant species Kosteletzkya pentacarpos is a promising species for phytostabilization of contaminated areas. In order to assess the role of the antisenescing phytohormone cytokinin in heavy metal resistance in this species, seedlings were exposed for two weeks to Cd (10 μM), Zn (100 μM) or Cd + Zn (10 μM + 100 μM) in the presence or absence of 50 mM NaCl and half of the plants were sprayed every two days with the cytokinin trans-zeatine riboside (10 μM). Zinc reduced the endogenous cytokinin concentration. Exogenous cytokinin increased plant growth, stomatal conductance, net photosynthesis and total ascorbate and reduced oxidative stress estimated by malondialdehyde in Zn-treated plants maintained in the absence of NaCl. Heavy metal induced an increase in the senescing hormone ethylene which was reduced by cytokinin treatment. Plants exposed to the mixed treatment (Cd + Zn) exhibited a specific hormonal status in relation to accumulation of abscisic acid and depletion of salicylic acid. Non-protein thiols (glutathione and phytochelatins) accumulated in response to Cd and Cd + Zn. It is concluded that toxic doses of Cd and Zn have different impacts on the plant behavior and that the simultaneous presence of the two elements induces a specific physiological constraint at the plant level. Salinity helps the plant to cope with heavy metal toxicities and the plant hormone cytokinin assumes key function in Zn resistance but its efficiency is lower in the presence of NaCl., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Salicylic acid (SA) is a phytohormone regulating immune responses against pathogens. SA and its derivatives can be found in diverse food products, medicines, cosmetics and preservatives. While salicylates have potential disease-preventative activity, they can also cause health problems to people who are hypersensitive. The current SA detection methods are costly, labor-intensive and require bulky instruments. In this study, a structure-switching aptamer-based nanopore thin film sensor was developed for cost-effective, rapid, sensitive and simple detection of SA in both buffer and plant extracts. SA is a challenging target for aptamer selection using conventional systemic evolution of ligands by exponential enrichment (SELEX) due to its small size and scarcity of reactive groups for immobilization. By immobilizing the SELEX library instead of SA and screening the library using a structure-switching SELEX approach, a high affinity SA aptamer was identified. The nanopore thin film sensor platform can detect as low as 0.1 μM SA. This is much better than the sensitivity of antibody-based detection method. This nanosensor also exhibited good selectivity among SA and its common metabolites and can detect SA in Arabidopsis and rice using only about 1 μl plant extracts within less than 30 min. The integration of SA aptamer and nanopore thin film sensor provides a promising solution for low-cost, rapid, sensitive on-site detection of SA., (Copyright © 2019 Elsevier B.V. All rights reserved.)

This work reports the synthesis of dual functional molecularly imprinted polymer (MIP)-modified organometal lead halide perovskite (CH 3 NH 3 PbI 3 ) and its application for photoelectrochemical (PEC) bioanalysis of salicylic acid (SA). Specifically, the CH 3 NH 3 PbI 3 was encapsulated into the MIPs via a simple thermal polymerization process on the indium tin oxide (ITO) glass, and the as-obtained MIPs/CH 3 NH 3 PbI 3 /ITO electrode was characterized by various techniques, which revealed that the MIPs could not only stabilize CH 3 NH 3 PbI 3 but also improve the electron-hole separation efficiency of CH 3 NH 3 PbI 3 under light illumination. In the detection of model analyte SA, the PEC sensor, with numerous amounts of recognition sites to SA, exhibited desirable performance in terms of good sensitivity, selectivity, stability, and feasibility for real sample analysis. This work not only featured the use of MIPs/CH 3 NH 3 PbI 3 for PEC detection of SA but also provided a new horizon for the design and implementation of functional polymers/perovskite materials in the field of PEC sensors and biosensors.

We reported two simple rhodamine-based colourimetric sensors for the first time which can selectively and sensitively detect salicylic acid (SA) under naked-eye detection. We proposed two distinctly different modes to elucidate the possible mechanism for monitoring SA. The rationally designed probes can be well exploited in signalling SA in living cell lines.

Insect attack is known to induce a high accumulation of volatile metabolites in tea ( Camellia sinensis). However, little information is available concerning the effect of insect attack on tea quality-related nonvolatile specialized metabolites. This study aimed to investigate the formation of characteristic nonvolatile specialized metabolites in tea leaves in response to attack by major tea insects, namely, tea green leafhoppers and tea geometrids, and determine the possible involvement of phytohormones in metabolite formation resulting from insect attack. Both tea green leafhopper and tea geometrid attacks increased the jasmonic acid and salicylic acid contents. The abscisic acid content was only increased under tea green leafhopper attack, perhaps due to special continuous piercing-sucking wounding. Tea green leafhopper attack induced the formation of theaflavins from catechins under the action of polyphenol oxidase, while tea geometrid attack increased the l-theanine content. Exogenous phytohormone treatments can affect the caffeine and catechin contents. These results will help to determine the influence of major tea pest insects on important tea quality-related metabolites and enhance understanding of the relationship of phytohormones and quality-related nonvolatile metabolite formation in tea exposed to tea pest insect attacks.

This work describes a simple screening protocol for quantification of carbasalate calcium derived metabolites, acetylsalicylic acid (ASA) and salicylic acid (SA), in animal and aquatic food matrices using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The analytes were extracted from porcine muscle, milk, egg, shrimp, eel, and flatfish using acetonitrile, with the addition of formic acid as well as trifluoroacetic acid, followed by liquid-liquid purification with saturated n-hexane. A reverse-phase analytical column was employed with a mobile phase comprising (A) 1 mM ammonium acetate in distilled water and (B) methanol to achieve the best chromatographic separation. Matrix-matched calibration curves (R 2  ≥ 0.9817) were constructed using six concentrations of 5, 10, 20, 30, 40, and 50 µg/kg in porcine muscle, milk, egg, shrimp, eel, and flatfish matrices. The calculated limits of quantification (LOQ) were 10 and 7 µg/kg, for ASA and SA, respectively. Recoveries of 67 to 102% with relative standard deviations (RSDs) of ≤9.0% (intra-day and inter-day) were obtained for all matrices at four spiking concentrations (5, 10, 20, and 50 µg/kg). The method was feasibly applied for monitoring market samples. In conclusion, the developed method is versatile, accurate, and precise for detecting and quantifying acetylsalicylic acid and salicylic acid residues in animal-derived foods meant for human consumption., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Objective and Significance: Methocarbamol (MET) and aspirin (ASP) are widely used as a muscle relaxant combination. The USP reports guaifenesin (GUA) and salicylic acid (SAL) as related substances and hydrolytic products of MET and ASP, respectively. This work aimed at developing and validating a simple and sensitive RP-HPLC method for the determination of both drugs as well as their related substances (at their pharmacopeial limits) in their bulk powders, laboratory prepared mixtures, and MET-ASP combined tablets. Methods and Results: Chromatographic separation was achieved in less than 9 min with the required resolution, peak symmetry, and accuracy on C 18 column using isocratic elution system of diluted acetic acid (pH 3.2): acetonitrile at the ratio of 79: 21, v/v, at a flow rate of 1 mL/min. Detection was achieved with photodiode array at 233 nm for MET, GUA, and SAL and at 273 nm for ASP. The developed method has been validated as per ICH guidelines and the calibration plots were linear over the concentration ranges of 2-150, 0.4-30, 25-450, and 0.2-27 μg/mL for MET, GUA, ASP, and SAL, respectively. Conclusion: The optimized method proved to be specific, robust and precise for the quality control of the studied drugs in pharmaceutical preparations to ascertain that their related substances are not exceeding the permitted pharmacopeial limits.

Salicylic acid (SA) is a class of trace pollutants widely presented in the environment belonged to pharmaceuticals and personal care products. It is difficult to remove SA by the traditional treatment processes because of its toxicity. In this paper, the degradation of SA by Mn-loaded Cu/Fe particle electrodes was studied. Firstly, the particle electrodes were prepared by impregnation-roasting method and then characterized by SEM, XRF and XRD. The diffraction peaks of Fe 2 O 3 and CuO in the XRD patterns of the particle electrodes which had the dense spherical particles were significantly increased and the content of CuO and Fe 2 O 3 increased by 1.9% and 3.6% respectively. Secondly, single factor experiments were carried out under conditions of cell voltage, electrolyte concentration, pH, HRT, inter-electrode distance and initial pollutant concentration. Under the optimum conditions of all the factors, the degradation rate of SA reached 76.9%. Then, HPLC and GCMS were employed to deduce the degradation pathways of SA by the TDE with Mn-particle electrodes (Mn-PETDE). Under the action of •OH, SA underwent decarboxylation and substitution reactions and then mineralized after the ring-opening reaction. All results demonstrated that this Mn-PETDE was effective for degradation of SA., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Elevated CO 2 alters C3 plant tolerance to insect herbivory, as well as the induction kinetics of defense hormones salicylic acid (SA) and jasmonic acid (JA), but the underlying physiological mechanism causing this response is not well understood. In principle, SA could be induced under elevated CO 2 by reactive oxygen signals generated in photosynthesis, ultimately influencing chemical defense. To test whether the effects of elevated CO 2 on C3 plant chemical defense against herbivorous insects are modulated by photosynthesis, Arabidopsis thaliana var. Col-0 plants were grown in two 2 × 2 × 2 nested factorial combinations of ambient (400 ppm) and elevated (800 ppm) CO 2 , and two dimensions of light regimes comprising intensity ('mild' 150 μmol E m -2  s -1 vs. 'low' light, 75 μmol E m -2  s -1 ) and periodicity ('continuous', 150 μmol E m -2  s -1 vs. 'dynamic', in which lights were turned off, then on, for 15 min every 2 h). Plants were challenged with herbivore damage from third instar Trichoplusia ni (cabbage looper). Consistent with experimental predictions, elevated CO 2 interacted with light as well as herbivory to induce foliar concentration of SA, while JA was suppressed. Under dynamic light, foliar content of total glucosinolates was reduced. Under combination of elevated CO 2 and dynamic light, T. ni removed significantly more leaf tissue relative to control plants. The observations that CO 2 and light interactively modulate defense against T. ni in A. thaliana provide an empirical argument for a role of photosynthesis in C3 plant chemical defense.

Phytoprostanes (PhytoPs) and phytofurans (PhytoFs) are oxylipins synthesized by nonenzymatic peroxidation of α-linolenic acid. These compounds are biomarkers of oxidative degradation in plant foods. In this research, the effect of environment and supplementation with salicylic acid (SA) on PhytoPs and PhytoFs was monitored by ultra-high-performance liquid chromatography coupled to electrospray ionization and triple quadrupole mass spectrometry (UHPLC-ESI-QqQ-MS/MS) on seven rice genotypes from Oryza sativa L. subsp. japonica. The plastic cover environment and spray application with 1 and 15 mM SA produced a reduction in the concentration of most of these newly established stress biomarkers [9-F 1t -PhytoP, ent-16-F 1t -PhytoP, ent-16- epi-16-F 1t -PhytoP, 9-D 1t -PhytoP, 9- epi-9-D 1t -PhytoP, 16-B 1 -PhytoP, 9-L 1 -PhytoP, ent-16( RS)-9- epi-ST-Δ 14 -10-PhytoF, ent-9( RS)-12- epi-ST-Δ 10 -13-PhytoF, and ent-16( RS)-13- epi-ST-Δ 14 -9-PhytoF] by 60.7% on average. The modification observed in the level of PhytoPs and PhytoFs differed according to the specific oxylipins and genotype, demonstrating a close linkage between genetic features and resistance to abiotic stress, to some extent mediated by the sensitivity of plants to the plant hormone SA that participates in the physiological response of higher plants to stress. Thus, in plants exposed to stressing factors, SA contribute to modulating the redox balance, minimizing the oxidation of fatty acids and thus the syntheis of oxylipins. These results indicated that SA could be a promising tool for managing the thermotolerance of rice crop. However, it remains necessary to study the mechanism of action of PhytoPs and PhytoFs in biochemical processes related to the defense of plants and define their role as stress biomarkers through a nonenzymatic pathway.

Preplanting foliar spray of salicylic acid (SA) (0.0, 5.0, and 10.0 μg/mL) to Solanum lycopersicum (L.) altered the metabolite profile of amino acids, γ-aminobutyric acid (GABA), and SA in leaf, root, and fruits. Free amino acid pools increased; bound amino acid pools reduced. In vegetative tissues, amino acid biosyntheses linked to osmo-compatibility (Pro, Leu, Val and GABA); N (Arg, Asn, Asp, Gln, and Glu); C (Pro, Ser, and Tyr); S (Cys) assimilation; stress tolerance (Ala, Gly, Hyp, His, Lys, Met, and Thr); and central metabolism (Phe, Trp, and Tyr) enhanced for 60-120 days. Concentrations of Ala, Arg, Gln, Gly, Leu, and Ser in leaf and of Asp, Cys, Glu, His, Hyp, Lys, Met, Pro, and Val in root predominated. In planta SA and GABA biosynthesis increased concurrently. SA affected GABA biosynthesis via Glu, Pro, and Arg metabolism. SA, GABA, Glu, and Pro were key canonical variables. This study first reported SA-induced metabolites promoting health (SA/GABA; Cys/Met) and palatability (Glu/Asp; Gln) in table tomato.

Plants can re-programme their transcriptome, proteome and metabolome to deal with environmental and biotic stress. It has been shown that the rhizosphere microbiome has influence on the plant metabolome and on herbivore behaviour. In the present study, Trichoderma gamsii was isolated from Arabidopsis thaliana rhizosphere soil. The inoculation of roots of Arabidopsis thaliana with T. gamsii significantly inhibited the feeding behaviour of Trichoplusia ni and affected the metabolome as well as the content of phytohormones in Arabidopsis leaves. T. gamsii-treated plant leaves had higher levels of amino acids and lower concentrations of sugars. In addition, T. gamsii-treated plant leaves had more abscisic acid (ABA) and lower levels of salicylic acid (SA) and indole-3-acetic acid (IAA) in comparison with the untreated plants. Furthermore, the inoculation with T. gamsii on different signalling mutants showed that the induction of defences were SA-dependent. These findings indicate that T. gamsii has potential as a new type of biocontrol agent to promote plant repellence to insect attacks., (© 2018 The Authors. Microbial Biotechnology published by John Wiley & Sons Ltd and Society for Applied Microbiology.)

We report the fabrication of an anion-exchange monolithic column in a stainless-steel chromatographic column (10 mm × 2.1 mm i.d.) using [2-(acryloyloxy) ethyl]trimethylammonium chloride as the monomer and ethylene dimethacrylate as the crosslinker. The prepared monolith was developed as the adsorbent for the on-line solid-phase extraction of salicylic acid in various animal-origin foodstuffs combined with liquid chromatography and tandem mass spectrometry. The monolith was characterized by using Fourier transform infrared spectroscopy, scanning electron microscopy, nitrogen adsorption analysis, and elemental analysis. Potential factors affecting the on-line solid-phase extraction and liquid chromatography with tandem mass spectrometry analysis were studied in detail. Under the optimized conditions, the total analysis time including cleanup and liquid chromatography with tandem mass spectrometry separation was 17 min. The developed method gave the linear range of 15-750 μg/kg, detection limits (S/N = 3) of 5 μg/kg, and quantification limits (S/N = 10) of 15 μg/kg. The recoveries obtained by spiking 10, 20, and 100 μg/kg of salicylic acid in the animal-origin food samples were in the range of 85.2-98.4%. In addition, the monolith was stable enough for 550 extraction cycles with the precision of peak area ≤11.6%., (© 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Preparation of novel salicylate-selective optical sensors (bulk optodes) was performed and applied successfully for salicylate determination in pharmaceutical formulations, Aspirin® and Aspocid®. t-butyl calix[4]arene ionophore was incorporated in a plasticized poly (vinyl-chloride) membrane containing the chromoionophore ETH5294 (O 1 ) or ETH7075 (O 5 ). The optical response to salicylate was due to size-selective extraction of salicylate from the aqueous solution to the optode bulk through formation of hydrogen bond accompanied by chromoionophore protonation, that resulted in the optical response at 680 or 540 nm for O 1 or O 5 , respectively. Reliable size-selectivity was measured for salicylate over other anions; The calculated selectivity coefficients of O 5 optode were found to be: -4.4, -2.0 and - 3.7 for iodide, benzoate and perchlorate, respectively. The hydrogen bonding mechanism and selectivity pattern were ensured and explained by IR and 1 H NMR spectroscopy. For the same purpose, a molecular recognition constant of β sal =10 0.043 was calculated using sandwich membrane method, and its small value ensured that hydrogen bonding interaction is responsible for the optode response. The detection limits of O 1 and O 5 in salicylate buffered solutions were 9.0 × 10 -5 and 8.9 × 10 -5  M with response times of 5 and 3 min, respectively, and with very good reversibility. The practical utility of the developed sensors was ensured by salicylate determination in Aspirin® and Aspocid®. Beyond the observed analytical performance, the present work aims not only to effectively apply Calixarene without derivatization, but also to estimate the strength of the size-dependent hydrogen bonding and comprehensively study the interaction mechanism., (Copyright © 2018 Elsevier B.V. All rights reserved.)

Tea plant (Camellia sinensis (L) O. Kuntze) respond to herbivore attack through large changes in defense related metabolism and gene expression. Ectropis oblique (Prout) is one of the most devastating insects that feed on tea leaves and tender buds, which can cause severe production loss and deteriorate the quality of tea. To elucidate the biochemicals and molecular mechanism of defense against tea geometrid (TG), transcriptome and metabolome of TG interaction with susceptible (SG) and resistance (RG) tea genotypes were analyzed by using UPLC-Q-TOF-MS, GC-MS, and RNA-seq technologies. This revealed that jasmonic acid was highly induced in RG, following a plethora of secondary metabolites involved in defense against TG could be induced by jasmonic acid signaling pathway. However, the constitutively present of salicylic acid in SG might be a suppressor of jasmonate signaling and thus misdirect tea plants against TG. Furthermore, flavonoids and terpenoids biosynthesis pathways were highly activated in RG to constitute the chemical barrier on TG feeding behavior. In contrast, fructose and theanine, which can act as feeding stimulants were observed to highly accumulate in SG. Being present in the major hub, 39 transcription factors or protein kinases among putative candidates were identified as master regulators from protein-protein interaction network analysis. Together, the current study provides a comprehensive gene expression and metabolite profiles, which can shed new insights into the molecular mechanism of tea defense against TG. The candidate genes and specific metabolites identified in the present study can serve as a valuable resource for unraveling the possible defense mechanism of plants against various biotic stresses., Competing Interests: The authors have declared that no competing interests exist.

The presence of pharmaceutical and personal care products and drugs of abuse (PPCPs) in wastewater treatment plants (WWTPs) indicates discharge of the effluent may not be suitable for the ecological balance of water ecosystems, such as wetlands. These PPCPs degrade water quality, considered as an ecosystem service (ES), provoking serious environmental impacts. Assessing the monetary value of PPCPs can be used as a proxy for environmental status of the ES of water quality (ESWQ). Considering PPCPs as non-desirable outputs of WWTPs, the shadow prices methodology has been implemented using directional distance function to measure the environmental avoided cost of removing salicylic acid (SA), methylparaben (MP), and THCOOH from WWTPs effluents discharged to Albufera Natural Park (Spain). The SA shows the highest shadow price (138.16 €/μg), followed by THCOOH (48.15 €/μg), and MP (30.66 €/μg). These values are interpreted as the environmental cost that would be avoided if SA, MP, and THCOOH were removed from WWTPs effluents. The non-parametric tests show that wastewater treatment technology, together with population equivalent (as a proxy of the size of urban areas) and seasonality are factors that influence shadow prices obtained. The approach used in this study highlights the use of PPCPs as status indicators of ESWQ quantified in monetary units. As a way to synthesize the essential concepts to implement the shadow prices approach, this study proposes a flow diagram to represent the relationship between all the factors involved in this work. The use of shadow prices methodology proves that removing SA, MP, and THCOOH is associated with a measurable improvement in the ESWQ of Albufera Natural Park. The findings of this study will be useful for plant managers in order to make decisions about the removal of PPCPs in WWTPs effluents., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Customized transcription factors that control gene expression in response to small molecules can act as endogenous molecular biosensors and are valuable tools for synthetic biology. We previously engineered the Escherichia coli regulatory protein AraC to respond to non-native inducers such as D-arabinose and triacetic acid lactone. Those prior studies involved the construction and screening of individual 4- or 5-site saturation mutagenesis libraries, followed by iterative rounds of positive- and negative fluorescence-activated cell sorting (FACS). Here we describe an improved screening platform and the isolation of several new and potentially useful AraC variants that respond to vanillin and salicylic acid. To increase throughput and reduce total screening time, selection steps were added to the sorting workflow. Two different site-saturation libraries and a random mutagenesis library were pooled together and >108 variants were subjected to iterative FACS and selection in search of variants responding to a panel of compounds. The new phenolic-sensing variants show responses >100-fold over background and are highly specific towards their target compound. The isolation of these variants further demonstrates the potential for engineering the AraC transcriptional regulatory protein for molecular sensing and reporting, and our improved screening system should prove effective in designing similar biosensors.

A field trial was conducted through 2015 and 2016 growing seasons to study the effect of nitrogen fertilizer sources and foliar spray with molybdenum (Mo), salicylic acid (SA) and their combination on tubers yield, some chemical constituents, nutrients uptake, nitrate accumulation and nitrate reductase activity in potato tubers. N source was added at a rate of 350 kg N ha -1 in five equal doses as two different forms, the first is urea and the second is ammonium sulfate plus calcium nitrate equally. SA was sprayed with three rates of 0, 75 and 150 mg l -1 . Also, Mo as ammonium molybdate was sprayed using three rates 0, 50 and 100 mg l -1 Mo. Both treatments of SA and Mo were applied separately as well as with each other, at three successive times 30, 50 and 70 days after planting of potato plants. Results indicated that the addition of 350 kg N ha -1 as ammonium sulfate and calcium nitrate equally caused a significant elevation (P > 0.05) in fresh weight, chlorophyll b, carotenoids, chlorophyll a, nitrate reductase activity, dry weight and NPK uptake by potato tubers compared with the same amount of nitrogen in the form of urea only. All the aforementioned characteristics were improved with increasing concentration of Mo and/or SA. The highest accumulation of nitrate was recorded under the addition of 350 kg N ha -1 as urea alone. The highest average of all the aforementioned characteristics was observed at the treatment of 350 kg N ha -1 as ammonium sulfate and calcium nitrate equally plus spraying with 100 mg l -1 Mo and 150 mg l -1 SA. In contrast, this treatment gave the lowest accumulation of nitrates in potato tubers.