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Phytic acid (IP6) and its degradation products lower myo-inositol phosphates exert different impacts on nutrient bioavailability and product quality characteristics. However, information regarding the occurrence of IP6 and its degradation products is scarce. In this work, simultaneous determination of IP6 and its degradation products in soybeans was developed, with emphasis on analysis by UPLC-MS/MS and a BEH Amide column both with hybrid surface technology. The retention and analyte/metal surface interactions issues were effectively addressed without ion-pairing reagents addition or derivatization. This method was applied to analyze soybeans from China. Total contents were 0.44–13.2 mg/g, and IP6 and its degradation product myo-inositol pentakisphosphate (IP5) were the predominant analytes, accounting for over 99%. Accession type significantly affected IP5 content, and landraces had significantly higher IP5 than cultivars. Geographically, the lowest IP6 was concentrated in the Huanghuaihai region. Significant correlations existed between IP6 and longitude, altitude, and annual cumulative sunshine hours. This study provides comprehensive insights into the IP6 and its degradation product profile in soybeans, which will benefit breeding soybeans based on specific requirements. • Analysis of IP1–6 was improved by UPLC-MS/MS and an amide column both with the HST • The retention was increased without ion-pairing reagents addition or derivatization • IP6 and IP5 were the predominant analytes, both accounting for over 99% • Landraces had significantly higher contents of IP5 than cultivars • IP6 was significantly correlated with certain geographical and climatic factors [ABSTRACT FROM AUTHOR]

Hibiscus sabdariffa L. (roselle) is a medicinal and edible plant which rich in anthocyanins with potent antioxidant properties. To enhance the stability of roselle anthocyanins, they were encapsulated in nanocapsules composed of carboxymethyl chitosan (CMC), chitosan hydrochloride (CHC), and β-lactoglobulin (β-Lg). In vitro simulated digestion assays evaluated the impact of various core-to-wall ratios and β-Lg concentrations on the bioaccessibility of seven anthocyanins. Nanocapsules with a core-to-wall ratio of 1:2 and β-Lg at 10 mg/mL exhibited the highest encapsulation efficiency (EE). Cyanidin-3-glucoside had the highest EE , while cyanidin-3-sambubioside showed the outstanding retention rate. Furthermore, simulated digestion experiments combined with molecular docking revealed that peonidin-3-glucoside and petunidin-3-glucoside likely interact with and bind to the outer β-Lg layer of the nanocapsules, increasing their release during in vitro digestion. This study demonstrates that encapsulating roselle anthocyanins in CMC, CHC, and β-Lg nanocapsules significantly enhances their bioaccessibility. Graphical abstract Roselle anthocyanins were encapsulated in nanocapsules using six different material concentrations. The encapsulation properties were evaluated to identify the optimal formulation with favorable particle characteristics and maximum bioaccessibility. During in vitro simulated digestion, changes in seven anthocyanins were monitored, highlighting cyanidin-3-sambubioside's high retention rate. Molecular docking analysis revealed that additional hydrophobic bonds enhance the binding of peonidin-3-glucoside and petunidin-3-glucoside to β-lactoglobulin in the capsule shell. [Display omitted] • C3G exhibited the highest encapsulation efficiency among quantified anthocyanins. • Hydroxyl groups in B-ring may increase the environmental sensitivity of D3G. • C3S showed the high retention rate during simulated digestion. • Hydrophobic bonds facilitate interaction of PEO and PET with β-lactoglobulin. [ABSTRACT FROM AUTHOR]

Alternaria toxins (ATs) are produced from Alternaria species that result in crop losses and harmful impacts on human health. A stable isotope dilution LC–MS/MS method was established to quantify four ATs in 15 food commodities: alternariol (AOH), alternariol monomethyl ether (AME), tentoxin (TEN), and tenuazonic acid (TeA). Based on systematically optimization of detection conditions and pre-processing steps, the limits of detection and limits of quantification of the four ATs ranged from 0.1 to 10 μg/kg and 0.2 to 30 μg/kg, respectively. The results showed that the recoveries of the four ATs were 72.0%–119.1%. The intra-precision and inter-precision ranged from 0.7% to 11.1% and 1.1% to 13.1%, respectively. The method was successfully applied to the determination of four ATs in 35 food samples, suggesting that this method could provide meaningful occurrence data to support the assessment of emerging ATs in food commodities. • A new method for the quantification of four Alternaria toxins on diverse food matrices was developed. • A solid phase extraction method was optimized on 15 food commodities screening. • The susceptibility of raw-food material and their derivatives to ATs contamination were confirmed. • High incidence and levels of TeA and TEN were found in 35 food samples screening. • TeA contents were high in dried wolfberry, dried chilli, sunflower seed, tomato sauces and wheat. [ABSTRACT FROM AUTHOR]

Both sedative and antipathogenic drugs are often found to be illegally used in aquaculture, but there is a lack of simultaneous monitoring methods. A method for simultaneously monitoring multiple prohibited drugs in various aquatic product samples was developed in this work, including fish, shrimp, crab, and shellfish. Sulfonic acid-functionalized magnetic graphitic carbon nitride (S-MGCN) was synthesized and validated to efficiently co-extract all targets (adsorption efficiency over 90.07%) through various adsorption mechanisms such as electrostatic interaction, hydrogen bonding, and π-π interaction while demonstrating good sample matrix purification ability (matrix effect below 13.60%). A new magnetic solid-phase extraction method based on S-MGCN was subsequently established. Coupled with UPLC-MS/MS, the detection limits were 0.030.075 μg /kg, and the recoveries ranged from 88.76% to 111.74% with the RSDs lower than 14.60%, indicating that the developed method has good sensitivity, accuracy, and precision. Further validation of its practicality was achieved through actual sample analysis. [Display omitted] • High throughput screening of multi-prohibited drugs in various aquatic samples was realized. • S-MGCN provides fast and efficient extraction of targets through multiple adsorption mechanisms. • S-MGCN exhibited good purification ability for sample matrix and reusability. • The accuracy and sensitivity of the method are equivalent to or better than existing methods. • The good practicality of the developed method was verified by testing actual samples. [ABSTRACT FROM AUTHOR]

Recently, amino acid derivatives gradually gained attention, but studies on N-lactoyl-leucine (Lac-Leu) and N-lactoyl-isoleucine (Lac-Ile) are limited. This study aims to explore the contributions of Lac-Leu and Lac-Ile to soy sauce. Lac-Leu and Lac-Ile were synthesized via enzymatic synthesis method catalyzed by Tgase. The mixed solutions containing Lac-Leu were found to have greater taste improvement than those containing Lac-Ile. Sensory evaluation indicated the sour, bitter, and astringent taste of Lac-Leu in water as well as its kokumi, astringent, and umami-enhancing taste in MSG solution. The taste threshold and umami-enhancing threshold of Lac-Leu measured by TDA and cTDA, respectively, were 0.08 mg/mL and 0.16 mg/mL. Molecular docking of Lac-Leu and Lac-Ile with the kokumi receptor CaSR and the umami receptors T1R1 and T1R3 indicated that Lac-Leu had higher affinities with receptors than Lac-Ile. These findings demonstrated the underlying contribution Lac-Leu made to soy sauce, indicating its potential to improve the flavor quality of soy sauce. • An enzymatic synthesis method of N-lactoyl leucine was established and optimized. • The taste characteristics of N-lactoyl leucine was investigated. • The thresholds of N-lactoyl leucine were determined by TDA and cTDA. • The taste mechanism of N-lactoyl leucine was explored by molecular docking. [ABSTRACT FROM AUTHOR]

A 3-step load-wash-elute solid-phase extraction tandem dedicated clean-up cartridge prior to UPLC-MS/MS for the simultaneous determination of bongkretic acid, isobongkretic acid and toxoflavin in food is presented in this work. The 3-step load-wash-elute SPE strategy with PRiME HLB, eliminating conditioning and equilibration, and coupled with dedicated purification cartridge, PriboFast MFC 336, was used as a tandem cartridge for sample pretreatment. Various sample pretreatment conditions including sample extractant, the tandem cartridge, the optimizatioin of PRiME HLB SPE conditions and PriboFast MFC 336 purification conditions, as well as MS/MS conditions and HPLC conditions were systematically investigated. Under the optimal experimental conditions, high sensitivity (LODs: 0.030–0.040 μg kg−1, LOQs: 0.090–0.12 μg kg−1), acceptable recoveries (83 %–96 %) and good precisions (r2 < 6.0 %) were obtained. The method was successfully applied to 90 food samples, bongkretic acid and isobongkretic acid were detected simultaneously in a dried black fungus, whereas toxoflavin was not detected in any of the samples. • Simultaneous detection of bongkretic acid, isobongkretic acid and toxoflavin in foods. • A possible cleavage mechanism of toxoflavin were presented and explained. • A 3-step load-wash-elute SPE cartridge tandem dedicated clean-up cartridge was used. • The method can be applied in relevant foods with satisfactory accuracy and precison. • For the first time, BA and IBA were detected simultaneously in a dried black fungus. [ABSTRACT FROM AUTHOR]

Co-extraction of multiple types of target substances is the key to achieve high throughput detection. In this work, PDA@MOF-808/PAN NFsM was prepared by co -modified polyacrylonitrile nanofiber membrane (PAN NFsM) with polydopamine (PDA) and metal-organic framework-808 (MOF-808), and its potential as a solid-phase extraction (SPE) adsorbent was investigated by using the most typical nine veterinary drug residues in eggs and chicken as model target substances. The results show that PDA@MOF-808/PAN NFsM could effectively co-extract all the target substances (adsorption efficiency ranged from 81.46 % to 96.78 %), and had good capability of sample matrix purification (matrix effect was lower than −15.26 %), so a new SPE method has been established. Combined with UPLC-MS/MS, the detection limits were 0.3 to 3.1 μg/kg, the recoveries were between 71.02 % and 106.48 %, and the relative standard deviations were lower than 12.03 %, indicating that the method has considerable good sensitivity, accuracy and precision. • High throughput screening of a variety of veterinary drugs in chicken and egg samples was achieved. • PDA@MOF/PAN NFsM provides fast and efficient extraction of targets through multiple adsorption mechanisms. • PDA@MOF/PAN NFsM exhibited good purification ability for sample matrix. • The accuracy and sensitivity of this method both meet the requirements of practical applications. • The good practicality of the developed method was verified by testing actual samples. [ABSTRACT FROM AUTHOR]

A novel analytical strategy was proposed to simultaneously quantify two advanced glycation end products (AGEs) including Nε-(Carboxymethyl)lysine (CML), Nε-(Carboxyethyl)lysine (CEL) and eight heterocyclic amines (HAs) including IQ, MeIQ, MeIQx, 4,8-DiMeIQx, 7,8-DiMeIQx, PhIP, Harman, and Norharman. The procedure was based on a two-step extraction, solid phase extraction (SPE) purification followed by ultra performance liquid chromatography tandem mass spectrometry. The established method showed a good linearity (R2 ≥ 0.9950), rapid processing time (8 min per sample), satisfactory recoveries (matrix spiked recoveries range from 72.2% to 119.6%) and precision (intra-day and inter-day RSDs were <19.3%). The limit of quantification (LOQ) and limit of detection (LOD) resulted to be between 0.05–15 ng/g and 0.2–50 ng/g, respectively. The validated technique was further applied to determine HAs and AGEs in eight stewed meat product samples consumed in Shanghai, with the amount of HAs and AGEs ranging from 2.851 to 18.289 ng/g and 118.158–543.493 ng/g, respectively. • The extraction, purification, and determination parameters were optimized. • UPLC-MS/MS was used to simultaneously analyze 8 HAs and 2 AGEs. • The method was with low solvent consumption and good precise. • This method was successfully applied in stewed meat products. [ABSTRACT FROM AUTHOR]

Tartary buckwheat, celebrated as the "king of grains" for its flavonoid and phenolic acid richness, has health-promoting properties. Despite significant morphological and metabolic variations in mature achenes, research on their developmental process is limited. Utilizing Liquid chromatography–mass spectrometry and atmospheric pressure matrix-assisted laser desorption/ionization mass spectrometry imaging, we conducted spatial-temporal metabolomics on two cultivars during achene development. Metabolic profiles including 17 phenolic acids and 83 flavonoids are influenced by both varietal distinctions and developmental intricacies. Notably, flavonols, as major flavonoids, accumulated with achene ripening and showed a tissue-specific distribution. Specifically, flavonol glycosides and aglycones concentrated in the embryo, while methylated flavonols and procyanidins in the hull. Black achenes at the green achene stage have higher bioactive compounds and enhanced antioxidant capacity. These findings provide insights into spatial and temporal characteristics of metabolites in Tartary buckwheat achenes and serve as a theoretical guide for selecting optimal resources for food production. • Spatial–temporal metabolomics of Tartary buckwheat achene were visualized. • Found 100 compounds, with flavonols as major achenes development flavonoids. • Flavonols showed space-specific distributions based on chemical modification. • The metabolic and bioactivity of achenes vary with species and development. • Immature black achenes own advantages in antioxidant ingredients and activity. [ABSTRACT FROM AUTHOR]

Carbonyl compounds are vital constituents that contribute to the flavor profile of alcoholic beverages. We examined 3-nitrophenylhydrazine as a derivatizing reagent for the measurement of 34 carbonyl compounds using UPLC−MS/MS. Adding formic acid and sodium acetate to the mobile phase significantly enhanced the detection limit of carbonyl compounds. The technique exhibited a notable extraction efficiency, yielding recovery percentages ranging from 83.6% to 117.1%, coupled with exceptional sensitivity, as evidenced by detection limits spanning from 0.07 μg/L to 4.80 μg/L. The relative standard deviation was <6.9%, indicating the precision and reliability of the analytical methodology. The method was verified by analyzing carbonyl compounds from red-fleshed kiwifruit wine. Furthermore, sensory assessment revealed that the amalgamation of tartaric acid, malic acid, and citric acid contributes to sour taste perception at sub-threshold concentrations through an additive interaction with supra-threshold non-volatile organic acids such as lactic acid and acetic acid. • A quantitative UPLC-MS/MS method for analysis of carbonyl compounds. • UPLC-MS/MS is more sensitive than GC for the detection of carbonyl compounds. • Acetic acid and lactic acid were presented with relatively high dose over thresholds. • Some organic acids were associated with sour taste at sub-threshold concentrations. [ABSTRACT FROM AUTHOR]

Advanced glycation end products (AGEs) and heterocyclic amines (HAs) are main harmful Maillard reaction products of meat products. Simultaneous quantification of both with high sensitivity, selectivity and accuracy remains a major challenge due to inconsistencies in their pre-treatment and instrumental methods and the different polarity of AGEs and HAs. We developed a method for the simultaneous determination of AGEs and HAs in roast/grilled meat by ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) using dynamic multiple reaction monitoring (D-MRM). The instrument parameters and pre-treatment method were optimized to achieve reasonably good separation and high response for the 11 target analytes within 8 min. From 10 to 200 ng/mL, the limits of detection (LODs) and limits of quantitation (LOQs) ranged from 0.3 to 5.5 μg/L and 0.9 to 6.3 μg/L, respectively, and the correlation coefficient (R2) was >0.99. It was acceptable to recoveries, standard deviations (RSDs), and matrix effects. Six types of roast/grilled meat samples were then tested using the developed method. [Display omitted] • A UPLC-MS/MS method was developed for simultaneous quantification of AGEs and HAs. • Optimization of UPLC-MS/MS conditions and sample preparation was discussed. • This method shows acceptable precision, recovery, sensitivity and matrix effects. • The distribution of AGEs and HAs differed in most types of roast/grilled meat. [ABSTRACT FROM AUTHOR]

[Display omitted] • A rapid UPLC-MS/MS method was optimized to detect 14 biogenic amines (BAs). • Daverine, histamine, tyramine, and putrescine were the dominant BAs in hairtail. • Vibrio could be the main BA-producing bacterium in deep-fried hairtail. • Deep-frying of hairtail was more recommended to inhibit BAs accumulation. Biogenic amines (BAs) produced by microbial decarboxylation of amino acids are crucial toxic nitrogenous compounds in fish. An optimized ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC–MS/MS) method with simple pretreatment was established to detect 14 BAs in both raw (control check, CK) and deep-fried (DF) hairtails. This method exhibited a good linear relationship with average recoveries of 73.3–120.0 % and relative standard deviations of 2.5–10.0 %, respectively. The total BAs in CK and DF hairtails decreased sharply to 338.2 and 25.3 mg/kg on the 9th day, respectively. Four BAs, including cadaverine (CAD), histamine (HIS), tyramine (TYR), and putrescine (PUT) accounted for 92.5–99.9 % of total BAs were selected as the dominant BAs. Bacterial analysis showed that the abundance of DF was relatively low. Further correlation analysis proved that Vibrio had a significant (p < 0.05) positive correlation with total BAs and could be the main BA-producing bacterium in DF hairtail. This work provides new evidence of the accumulation of BAs in refrigerated hairtail. [ABSTRACT FROM AUTHOR]

[Display omitted] • Construction of a sugar-smoking model reaction to study the primary pathways of sugar-smoking pigment formation. • The primary source of 5-HMF was identified as fructose resulting from the cleavage of sucrose at 330 °C. • The primary pathway for the formation of 5-GGMF was attributed to the intermolecular dehydration of 5-HMF and glucose at 150 °C. • The 5-HMF-glucose model reaction product displayed stronger radical scavenging abilities. The present study aimed to elucidate the pathway of pigment formation and identify the source of antioxidant activity during sugar smoking. Building upon previous research, this investigation replicated the sucrose cleavage process involved in sugar-smoking through model reactions to obtain distinct model reaction products. The products were analyzed using various techniques such as ultraviolet–visible spectrometry, Fourier-transform infrared spectroscopy, high-performance liquid chromatography, and high-performance liquid chromatography-tandem mass spectrometry. The findings revealed that the pyrolysis of sucrose at 330 °C yielded glucose and fructose, with fructose pyrolysis producing significantly more 5-HMF than glucose. Moreover, the antioxidant capacity of 5-HMF was found to make a substantial contribution. The primary source of 5-HMF was identified as fructose resulting from the cleavage of sucrose at 330 °C, while the primary pathway for the formation of the sugar-smoking pigment 5-GGMF was attributed to the intermolecular dehydration of 5-HMF and glucose at 150 °C. [ABSTRACT FROM AUTHOR]

[Display omitted] • A recombinant full-length isotope-labelled tropomyosin was expressed with high purity and isotope labeling ratio. • An absolute LC-MS/MS quantification assay was developed for shrimp tropomyosin in complex food matrices. • The limits of quantification for tropomyosin were 1–10 μg/g. • This method was successfully applied to the accurate quantification of tropomyosin in real samples. The carryover of trace allergens in complex food matrices poses challenges for detection techniques. Here, we demonstrate an accurate UPLC-MS/MS quantification assay for the shrimp allergen tropomyosin with a full-length isotope-labelled recombinant tropomyosin (TM-I) internal standard in complex food matrices. The TM-I, expressed based on the SILAC technique, exhibited a high isotope labelling ratio (>99%), purity, and alignment with the natural sequence. This method determined the tropomyosin ranging from 0.2 to 100 ng/mL. Mean recoveries ranged from 89 to 116%, with intra- and inter-day RSDs below 12%, for three signature peptides across three types of commercially processed food matrices. The limits of quantitation were 1 μg/g in pop food and sauce, and 10 μg/g in surimi product, respectively. This study supports the use of recombinant full-length isotope-labelled proteins rather than stable-isotope labelling peptides as internal standards to achieve more accurate quantitation of food allergens as the digestion error is corrected. [ABSTRACT FROM AUTHOR]

• EVOO composition is affected more by storage time than agronomic or technological factors. • EVOO composition changed most in the early storage period and when room temperature increased. • K 270 is a clear marker of EVOO deterioration during storage. Extra virgin olive oil (EVOO) quality and composition are mainly affected by genetics, agronomic and technological parameters, undergoing further modifications during storage. In this work, a chemometric approach was applied to study the impact of olive maturity, malaxation time/temperature, and oil storage on the quality and compositional parameters of Arbequina EVOO (basic quality indices, volatile and sensory profiles, contents in phenolic compounds, squalene, vitamin E and fatty acids). Storage emerged as the most influential factor, followed by olive maturity and malaxation temperature, while malaxation time had almost no effect. Storage at room temperature had a significant impact on the phenolic profile and quality parameters, mainly the peroxide value and K 270. The determination of K 270 , an indicator of secondary oxidation products, was relevant to analyze the effect of storage conditions. Volatile compounds and fatty acids were good markers of ripeness, and the volatile profile was highly affected by malaxation temperature. [ABSTRACT FROM AUTHOR]

[Display omitted] • A new method for the analysis of 15 pyrrolizidine alkaloids (PAs) and their N -oxides (PANOs). • The method for analysis of 15 PAs/PANOs in soil of tea garden was first developed. • PAs/PANOs in tea were derived from the weeds in tea garden. • Intermedine- N -oxide was the highest PANO in weeds. Pyrrolizidine alkaloids (PAs) and their N -oxides (PANOs) are novel contaminants in tea. However, the source of PA/PANO contamination in tea remains unclear. In this study, 15 PAs/PANOs were extracted from plant samples (tea, fresh tea leaves, and weeds) with 0.1 M sulfuric acid and from soil with 0.1 M sulfuric acid methanol after adjusting soil acidity with 0.1 M trisodium citrate. Satisfactory recoveries of PAs/PANOs from four different matrices at 0.02, 0.1, and 0.5 mg kg−1 was 72%–114% with relative standard deviations (RSD) of 0.03%–16%. Seven out of 15 PAs/PANOs were detected in tea purchased from the local market ranging from undetected to 96.2 μg kg−1. Thirteen, three, and four PAs/PANOs were detected in weeds, fresh tea leaves, and soil, respectively. Based on the types of PAs/PANOs detected in the three matrices, it was preliminarily speculated that PAs/PANOs in tea originated from weeds in the tea garden. [ABSTRACT FROM AUTHOR]

• Changes in non-volatile metabolites and antioxidants were investigated in EMD. • More metabolites were found in Koji and the first 5-day post-fermented sample. • Flavonoids were the largest class of differential metabolites. • The antioxidant capacity of EMD gradually increased with the fermentation time. • The antioxidant capacity of EMD was closely related to flavonoid metabolites. This study investigated the non-volatile metabolites and antioxidant activity of Douchi, an edible mushroom by-product. A total of 695 non-volatile metabolites were detected using UPLC-MS/MS-based metabolomics analysis, and the greatest impact on metabolite composition was observed during Koji-making and the first 5 days of post-fermentation. Throughout the fermentation process, 366 differential metabolites were identified, with flavonoids being the most prominent followed by amino acids and their derivatives, which were found to be important for the quality of edible mushroom by-product Douchi (EMD). The antioxidant capacity of EMD significantly increased with the longer fermentation time, which might be associated with the conversion of isoflavone glycosides to aglycones, amino acids and their derivatives, free fatty acids, group A saponins, and phenolic acids. These findings suggested that different fermentation phases of EMD significantly affected the non-volatile metabolite profile and antioxidant capacity. [ABSTRACT FROM AUTHOR]

[Display omitted] • A two-step pretreatment was developed for simultaneous extraction of 17 TPHs. • 17 TPHs were simultaneously quantitated by UPLC-MS/MS within 7 min. • Good quantification accuracy, precision, and recovery were achieved. • The method was applied to high starch/protein/fat/sugar food products. • PCA was performed to visualize the association between TPHs and food matrices. A two-step pretreatment and UPLC-MS/MS-based method was established to extract and determine 17 thermal processing hazards (TPHs) simultaneously. The first step was to extract acrylamide (AA), 5-hydroxymethylfurfural (HMF) and free heterocyclic amines (HAs). The bound HAs and advanced glycation end products (AGEs) were released by acid hydrolysis in the second step. A fairly good separation was achieved within 7 min. Almost all TPHs showed high correlation coefficients (R2 >0.999) in their respective linear ranges. The accuracy ranged from 98.13 to 100.96%. LODs and LOQs were in the range of 0.01–0.89 µg/L and 0.02–2.96 µg/L, respectively. The method was successfully applied to four representative food products, including high-starch, high-protein, high-fat and high-sugar foods, showing acceptable recoveries, intra-day and inter-day precisions. Moreover, PCA was performed to visualize the association between TPHs and food matrices. The developed method provided technical support for the formation and control researches of TPHs. [ABSTRACT FROM AUTHOR]

• The CAA of different honeys were evaluated comprehensively. • The CAA markers in honey were firstly explored based on the QCAR. • The antioxidant research on fennel honey was firstly investigated. • Phenolic acids, flavonoids and free amino acids in different honeys were analyzed. • Isosakuranetin, cryptochlorogenic acid and methionine were firstly found in honey. Antioxidant molecules in honey contributed to various biological effects, but antioxidant components markers in honey are required to be investigated further. Phenolic compounds, flavonoids and free amino acids were analyzed using UPLC-MS/MS and HPLC-FLD from 39 honey samples, in which fennel honey was firstly investigated. Based on the quantitative composition-activity relationship, the cellular antioxidant activity (CAA) assay of various honeys is closely related with the interaction of some phenolic compounds (isoferulic acid, 3,4-dihydroxy benzoic acid, 4-hydroxy benzoic acid, chlorogenic acid, caffeic acid, gallic acid, cryptochlorogenic acid, p -coumaric acid, salicylic acid), flavonoids (isosakuranetin, sakuranetin, pinocembrin, vitexin, taxifolin, galangin, luteolin, chrysin) and free amino acids (Tyr, Gly, Ile, Glu, Val, Phe, Leu, Asp, His, Pro, Ala). The results would be beneficial for the understanding of the nutritional values, exploitation and utilization of honeys with different floral origins, further contributable to the market development and consumption choice of honey. [ABSTRACT FROM AUTHOR]

• A novel method for pesticides and mycotoxins determination in wine was developed. • Both classes of contaminants were determined simultaneously via direct injection technique. • Sample preparation performed in three steps: centrifugation, dilution and filtration. • Validation performed following the criteria established by SANTE document. A simple and rapid method for simultaneous determination of pesticides and mycotoxins in red wine is presented. Sample preparation approach, called direct injection, consists of a sequence of only three steps: centrifugation, dilution and filtration. The analysis of extracts were performed by UPLC-MS/MS for determination of pesticides and mycotoxins. The method was assessed for linearity, limits of detection and quantification, matrix effects, selectivity, accuracy and precision. For recovery experiments, mycotoxins were divided in two groups according to their sensitivity in the UPLC-MS/MS system. More than 80% of the mycotoxins were reliably quantified at the lowest spike level studied (1 μg kg−1 for group 1 and 50 μg kg−1 for group 2). From the 185 evaluated pesticides, 144 showed acceptable results at 10 μg kg−1, the lowest spiked level. Matrix effects were, in most of the cases, negative, and that was observed for both pesticides and mycotoxins. [ABSTRACT FROM AUTHOR]

Highlights • Eight (five free and seven bound) HAs at levels up to hundreds of ng/g were detected in sausage. • Smoking could increase HAs to more than twice levels found in baked sausages. • At higher baking temperatures, lower levels of HAs were found in baked sausages. • At higher smoking temperatures, higher levels of HAs were found in smoked sausages. • The highest total HAs was 422 ± 17.5 ng/g in sausages smoked at 60 °C. Abstract We used an UPLC-MS/MS method to investigate the effects of smoking or baking on the formation of heterocyclic amines (HAs) in sausage processing. We used principal component analysis (PCA) to differentiate the chemical composition, pH and colour of the processed sausages. We detected and quantified eight types of HAs (PhIP, DMIP, Phe-P-1, IQ[4,5- b ], 7,8-DiMeIQx, AαC, harman and norharman) in sausages, finding total HA concentrations as high as 422 ± 17.5 ng/g. Higher smoking temperatures led to higher concentrations of total HA in smoked sausages (330 ± 8.19 to 422 ± 17.5 ng/g). On the contrary, higher baking temperatures created lower total HA concentrations in baked sausages (ranging from 139 ± 9.83 to 306 ± 0.92 ng/g). Our results demonstrated that HAs are produced even at low temperatures, which means that HAs should be controlled during sausage processing to minimise their formation. [ABSTRACT FROM AUTHOR]

Highlights • A new method was developed for the analysis of mycotoxins in beer. • The method allows the identification and quantification of 23 mycotoxins. • A QuEChERS extraction involving sample preconcentration was developed. Abstract A new method based on a QuEChERS extraction followed by the ultra-high liquid chromatography tandem mass spectrometry (UPLC-MS/MS) detection has been developed for the analysis of mycotoxin in beer. The method allows the identification and quantification of 23 mycotoxins with different chemical characteristic including regulated, emerging and masked compounds. A sample treatment procedure involving a QuEChERS extraction and dispersive solid-phase clean-up steps was applied. This protocol involves a new approach based on a sample concentration before the extraction. The method was in-house validated in terms of limits of detection (LODs), limits of quantification (LOQs), linearity, repeatability and recoveries. For most compounds, recoveries ranged from 70% to 110% with LOQs (from 0.038 to 30.43 µg/L) lower than the maximum residue levels established in European regulations. In general, acceptable performance characteristics were obtained fulfilling the current legislation. Therefore, the proposed method is appropriate for routine analysis of beer. [ABSTRACT FROM AUTHOR]

Graphical abstract Highlights • Extraction optimized using tea sprayed with multiple pesticides in the field. • Additives to LC-MS mobile phase compared for multiple classes of pesticides. • Matrix effects of four agri-products cleaned-up with PVPP were compared. • Dilution aided detection of multiple classes of residues in polyphenol-rich foods. Abstract An efficient method for the rapid extraction and clean-up of 20 pesticide residues from polyphenol-rich agricultural samples (tea, apple, broccoli, and shallot) for analysis by UPLC-MS/MS was developed. Following extraction, PVPP was used to precipitate polyphenols, supernatant was diluted to minimize matrix effects. Homogenized samples were vortexed in acetonitrile prior to cleanup with a combination of PVPP (150 mg), PSA (50 mg) and GCB (10 mg). Supernatant (1 mL) was filtered and diluted 10-fold before analysis. In 4 agricultural products that usually produce high interference, the matrix effects were overcome for all pesticides expect in green and oolong tea for acephate, omethoate, dinotefuran and nitenpyram. Mean recoveries ranged from 73% to 106%, and RSD ≦ 13%. Limits of quantification ranged from 0.01 to 0.02 mg kg−1. PVPP as one of excellent QuEChERS material combined with dilution was verified as a promising method for multiple pesticide residues analysis in complex matrices. [ABSTRACT FROM AUTHOR]

Highlights • An efficient UPLC-MS/MS method for the determination of perchlorate in tea is established. • The comparison of purification efficiency between Cleanert PWAX SPE and others is done. • Perchlorate residue in dark tea is found higher than that in black tea or green tea. • Perchlorate in tea accumulates along with the growth of tea leaves. • Other pollutant sources of perchlorate should exist during planting process. Abstract Perchlorate causes great health concerns for its inhibition on the iodide intake of human. However, the contamination pattern of perchlorate in tea remains unclear although tea is substantially consumed worldwide. Thus, the present study established an efficient method using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) in combination with external standard method, and further lucubrated the contamination level of perchlorate in made tea, fresh tea leaves, along with the waters and soils from tea gardens. Fresh tea leaves with higher maturity generally contains more perchlorate. The observation explains well why the residual of perchlorate in dark tea is generally higher than that in black tea or green tea from the perspective of raw material. In consideration of the ubiquitous existence of perchlorate in waters and soils from tea gardens, perchlorate might accumulate in tea leaves via soil. This study not only provides an alternative quantification method of perchlorate when the isotope internal standard is out of stock, but also illuminates the contamination pattern of perchlorate in tea from planting process. [ABSTRACT FROM AUTHOR]

Graphical abstract Highlights • A reliable mass spectrometric method was developed for serotonin in nuts. • Optimization of extraction procedure from complex nut matrices was performed. • Serotonin content of wide range of edible nuts were reported for the first time. • Serotonin content of nuts and nut products ranged from 0.03 to 155 µg/g fresh weight. Abstract An ultra performance liquid chromatography-mass spectrometry (UPLC-MS/MS) method was developed for the determination of serotonin in raw and roasted nuts (almond, Brazil nut, cashew, chestnut, coconut, hazelnut, Macadamia nut, pecan, peanut, pine nut, pistachio and walnut) as well as nut products (nut containing snack bars, chocolate and spreads) for the first time. Water extraction without prior defatting was performed to leach serotonin from complex matrices of nuts. Mean recoveries ranged from 64.2 ± 9.6 to 94.7 ± 20.1%. Limit of detection and limit of quantification were between 0.4 and 2.3 and 1.0–7.4 ng/g, respectively. Repeatability and reproducibility values were below 2%. Serotonin content of nuts ranged from 0.05 ± 0.01 (pine nut) to 155 ± 57.0 µg/g (walnut) in raw nuts while it was between 0.03 ± 0.00 (Macadamia nut) and 15.3 ± 1.27 µg/g (pecan) in roasted nuts. Serotonin in nut products was found to range from 0.09 ± 0.00 to 8.99 ± 0.92 µg/g, depending on the nuts they contain. [ABSTRACT FROM AUTHOR]

In this report, a UPLC–ESI–MS/MS method for the simultaneous determination of aflatoxins, ochratoxin A, zearalenone, deoxynivalenol, fumonisins, T-2 and HT-2 toxins, fusarenone X, diacetoxyscirpenol, and 3- and 15-acetyldeoxynivalenol in feedstuffs was developed. A quadrupole-time-of-flight mass spectrometer detector (QTOF–MS) operating in full scan mode was combined with the UPLC–ESI–MS/MS system to confirm the identity of detected mycotoxins and to identify other possible microbial metabolites occurring in samples. Sixty-two feed samples from the Spanish market were analyzed. Extraction of metabolites was carried out with acetonitrile-water-formic acid (80:19:1, v/v/v). Method detection and quantification limits and performance criteria set by Commission Regulation (EC) No 401/2006 were fulfilled. Relatively high levels of the main regulated mycotoxins and presence of non-regulated mycotoxins in feed samples were found. This is the first study in which mycotoxins and other microbial metabolites occurring in feed are studied using a UPLC–QTOF–MS system being therefore a reference report. [ABSTRACT FROM AUTHOR]

An accurate, reliable and fast multi-residue, multi-class method using ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) was developed and validated for simultaneous determination and quantification of 24 pharmacologically active substances of three different classes (Quinolones including fluoroquinolones, sulphonamides and tetracyclines) in aquaculture shrimps. Sample preparation involves extraction with acetonitrile containing 0.1% formic acid and followed by clean up with n -hexane and 0.1% methanol in water by UPLC-MS/MS within 8 min. The method was validated according to European Commission Decision 2002/657. Acceptable values were obtained for linearity (5–200 μg kg −1 ), specificity, Limit of Quantification (5–10 μg kg −1 ), recovery (between 83 and 100%), repeatability (RSD < 9%), within lab reproducibility (RSD < 15%), reproducibility (RSD ≤ 22%), decision limit (105–116 μg kg −1 ) and detection capability (110–132 μg kg −1 ). The validated method was applied to aquaculture shrimp samples from India. [ABSTRACT FROM AUTHOR]

An accelerated solvent extraction (ASE) with in-cell clean-up method coupled to ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed to determine 21 antibiotics in sea cucumber. The analytes include 10 sulfonamides, 4 fluoroquinolones, 3 amphenicols, 2 beta-lactams, 1 lincosamide and trimethoprim. Optimal parameters of ASE method were obtained at 80 °C, 1 static cycle of 5 min with methanol/acetonitrile (1/1, v/v) using 2 g of C18 as adsorbent. Recoveries at 50.1–129.2% were achieved with RSD under 20%. Method detection limits ranged from 0.03 to 2.9 μg kg −1 . Compared to the reported ultrasound-assisted extraction method, the proposed method offered comparable extraction efficiency for sulfonamides from sea cucumber, but higher for other categories of antibiotics. This validated method was then successfully applied to sea cucumber samples and 9 antibiotics were detected with the highest concentration up to 57.7 μg kg −1 for norfloxacin. [ABSTRACT FROM AUTHOR]

A reliable UPLC–MS/MS method with high sensitivity was developed and validated for the determination of virginiamycin M1 in muscle, fat, liver, and kidney samples of chicken and swine. Analytes were extracted using acetonitrile and extracts were defatted by N -hexane. Chromatographic separation was performed on a BEH C18 liquid chromatography column. The analytes were then detected using triplequadrupole mass spectrometry in positive electrospray ionization and multiple reaction monitoring mode. Calibration plots were constructed using standard working solutions and showed good linearity. Limits of quantification ranged from 2 to 60 ng mL −1 . [ABSTRACT FROM AUTHOR]

Molecularly imprinted porous polymer microspheres selective to Alternaria mycotoxins, alternariol (AOH) and alternariol monomethyl ether (AME), were synthesized and applied to the extraction of both mycotoxins in food samples. The polymer was prepared using 4-vinylpiridine (VIPY) and methacrylamide (MAM) as functional monomers, ethylene glycol dimethacrylate (EDMA) as cross-linker and 3,8,9-trihydroxy-6 H -dibenzo[ b,d ]pyran-6-one (S2) as AOH surrogate template. A molecularly imprinted solid phase extraction (MISPE) method has been optimized for the selective isolation of the mycotoxins from aqueous samples coupled to HPLC with fluorescence (λ ex = 258 nm; λ em = 440 nm) or MS/MS analysis. The MISPE method was validated by UPLC–MS/MS for the determination of AOH and AME in tomato juice and sesame oil based on the European Commission Decision 2002/657/EC. Method performance was satisfactory with recoveries from 92.5% to 106.2% and limits of quantification within the 1.1–2.8 µg kg −1 range in both samples. [ABSTRACT FROM AUTHOR]

The in vivo determination of selenomethionine (SeMet) converted from selenium-enriched yeast (SeY) rather than the determination of in vitro hydrolyzed SeMet is a better parameter for the evaluation of SeY quality. A UPLC–MS/MS method was developed for the quantification of SeMet in rat plasma and the oral bioavailability of SeMet converted from SeY in rats. After a simple extraction with perchloric acid, SeMet and the internal standard methylselenocysteine (MSC) were separated on a C18 column with isocratic elution of water:acetonitrile:formic acid (99:1:0.1, v / v / v ) and detected in the multiple reaction monitoring mode. The method was accurate (92.6–104.3%) and precise (1.8–11.0%), and the recovery was 79.4–95.4%. It was successfully applied to pharmacokinetic and bioavailability studies of SeY in rats following the intravenous administration of SeMet and intragastric administration of SeY. SeMet in vivo , converted from SeY, is reported for the first time, and the results suggested that the SeY bioavailability in rats is 87%. [ABSTRACT FROM AUTHOR]

This study evaluated the inhibitory effects of Sichuan pepper ( Zanthoxylum bungeanum ) and sanshoamide extract on the formation of heterocyclic amines (HAs) in grilled beef patties. The following major HAs were detected and quantified: imidazopyridine (2-amino-1-methyl-6-phenylimidazo[4,5- b ]pyridine, PhIP), imidazoquinoxalines (2-amino-3-methyl-3H-imidazo[4,5- f ]quinoxaline, IQx; 2-amino-3,8-dimethylimidazo[4,5- f ]quinoxaline, MeIOx; 2-amino-3,4,8-trimethyl-3H-imidazo[4,5- f ]quinoxaline, 4,8-DiMeIQx) and β-carbolines (9H-pyrido[3,4- b ]indole, norharman; 1-methyl-9H-pyrido[3,4- b ]indole, harman). The rates of PhIP, IQx, MeIQx and 4,8-DiMeIQx were inhibited significantly by 82%, 61%, 28% and 79%, respectively, in patties treated with a low-concentration of pepper (0.5%), and by 27%, 45%, 44% and 26%, respectively, following treatment with a low-concentration sanshoamide extract (0.005%). All inhibition rates exceeded 70% at pepper and sanshoamide extract concentrations of 1.0% and 0.010%, respectively. Harman and norharman could be significantly (p < 0.05) enhanced by the addition of all concentrations of Sichuan pepper, however, sanshoamide extract had no significant (p > 0.05) effect on them, although 0.005% of the extract could slightly increase the formation of them. Notably, significant correlations were observed between the HA inhibition rates and pepper or sanshoamide extract concentrations, especially for PhIP (r = 0.87, p = 2.30E−3), IQx (r = 0.99, p = 5.04E−7) and 4,8-DiMeIQx (r = 0.88, p = 1.96E−3). These results indicate that Sichuan pepper and sanshoamide extract could inhibit the formation of carcinogenic HAs during thermal preparation of protein-rich foods, and therefore might reduce the risk of chronic diseases associated with the long-term intake of HA-containing food products. [ABSTRACT FROM AUTHOR]

Strip with three test lines was developed for semi-quantitative and quantitative determination of deoxynivalenol through four visual detection thresholds and smart platform. The results indicated that this type of strip could reveal DON content visually and quantitatively with high accuracy. [Display omitted] • A three test lines strip was developed for quantitative detection of DON. • Four visual detection thresholds for quantitative determination were obtained. • 35 wheat samples with DON content from 45 µg/kg to 2841 µg/kg were detected. • The developed method was confirmed by UPLC-MS/MS. • The results of multiline strip were compared with that of traditional strip. Lateral flow strip was widely used and their qualitative and quantitative performance was in continuous improvement. However, the traditional strip was in a single-test-line format, which restricted operators to making a semi-quantitative judgment around a desired threshold concentration. Herein, a single strip with three test lines (TTLS) was developed for the semi-quantitative and quantitative determination of deoxynivalenol (DON). Four visual detection thresholds were obtained under optimized conditions and 35 wheat samples with DON content from 45 µg/kg to 2841 µg/kg were used to verify the method. The detection results were compared with that of the traditional strip and UPLC-MS/MS. In a three-test-line format, TTLS could reveal at least 200, 500, 1000, and 2000 µg/kg DON existed in different samples by the naked eye. The agreement analysis and statistical results indicated the new TTLS can be used as a useful tool for quantitative detection of DON with wide dynamic range. [ABSTRACT FROM AUTHOR]

• The carotenoids in the waste apricot flesh were extracted into the corn oil. • Extraction conditions of ultrasound-assisted corn oil extraction were optimized. • The highest content of carotenoids in corn oil extracts was phytoene. • Corn oil extracts as frying medium can improve the color (a*) of French fries. The valorization of waste apricot flesh (WAF) can solve environmental and economic problems, and also meets the demand for natural pigments. Therefore, the aim of this paper was to recover carotenoids from WAF, to determine the type and content of carotenoids in the extracts and to explore the potential of the extracts for food industry applications. The extraction conditions were optimized. The total carotenoids content (TCC) was 42.75 mg/100 g dried weight under the optimized conditions: Time: 60 min, Temperature: 41.53℃, Power: 200 W, Liquid to solid (LS) ratio: 0.10 g/mL. The highest content of carotenoids in the corn oil extracts (COE) was phytoene. Color of COE under high temperature was investigated. Carotenoids in the COE were degraded at high temperatures. The a* of fries fried by COE was 7.31 times higher than that of corn oil. This study provides guidance for the green recovery of carotenoids and valorization of WAF. [ABSTRACT FROM AUTHOR]

• A UPLC-MS/MS method was developed and verified to detect albendazole in citrus. • Evaluated storage stability of albendazole on whole citrus and citrus pulp. • Field dissipation and terminal residue of albendazole in citrus were investigated. • Persistence of the albendazole in citrus was low, with DT50 values lower than 18 days. • The chronic dietary risk of albendazole on citrus are acceptable to consumer. Albendazole is a broad-spectrum fungicide that shows great potential in controlling fungal diseases in citrus. To quantify the dissipation behavior, residue distribution, and dietary risk of albendazole in citrus, we developed an UPLC-MS/MS analysis protocol. The average recovery rate of albendazole in whole citrus and citrus pulp ranged from 74 to 105% with an RSD of 3 to 8%, and a limit of quantification of 0.01 mg kg−1. The degradation half-lives were 2.8–3.0 and 5.7–17.0 days in whole citrus and citrus pulp, respectively, and the final residues of albendazole were <0.059 mg kg−1 with a risk quotient of <1. This study not only demonstrates that the dietary risk of albendazole in citrus is negligible, but also provides empirical data to establish the maximum residual limit (MRL) for the safe application of albendazole in citrus orchards to meet the requirements for food safety as well as international trade. [ABSTRACT FROM AUTHOR]

[Display omitted] • Metabolomics revealed that drying affects flavonoids in sea buckthorn berries. • The flavonoid content increased and antioxidant capacity decreased after drying. • Hot air drying and infrared drying had distinct effects on flavonoid compounds. Flavonoids are major nutrients in sea buckthorn berries. However, the effects of drying methods on flavonoids in sea buckthorn berries are unclear. In this study, ultra-performance liquid chromatography and metabolomics were adopted to analyse the effects of hot air drying (HAD) and infrared drying (IRD) on flavonoid compounds and antioxidant capacity in sea buckthorn berries. In total, 97 metabolites belonging to 12 classes were identified, including 26 flavones, 23 flavonols, and 11 flavanones. Additionally, 32 differential metabolites were identified among groups. Isorhamnetin and quercetin contents increased in response to HAD and IRD, while (-)-epigallocatechin and (-)-gallocatechin contents decreased. Differential metabolism of flavonoid compounds occurred mainly via the flavonoid biosynthesis and secondary metabolite biosynthesis pathways. Flavonoid compound degradation might be associated with antioxidant activity during drying. This study elucidated the effect of drying on nutritional components of sea buckthorn berries and may guide the improvement of quality during food processing. [ABSTRACT FROM AUTHOR]

Occurrence of Rhodamine B (RhB) contamination in paprika caused by agricultural materials during the vegetation process has been reported. It may transfer during the process of active compounds extraction, and eventually exist in final products. Herein, the re-distribution of RhB during the extraction process was assessed in terms of RhB contents, as well as mass, color value and capsaicinoids yield of each process. Results revealed that natural RhB contamination at 0.55–1.11 µg/kg originated from raw paprika fruit then transferred with the extraction proceeded. About 95.5% of RhB was found in red oleoresin. After separation of red oleoresin, 91.6% of RhB was remained in capsicum oleoresin, only 3.7% in paprika red. These results were consistent with total capsaicinoids recovery of each product. The RhB levels in edible capsicum oleoresin in our present study at 0.01–0.34 µg/kg did not exceed the legal limits established by the European Union. [ABSTRACT FROM AUTHOR]

Varietal thiols are key aroma compounds in wine issued from multiple and complex origins. Several precursor families have been identified in grapes and must and have been widely studied. But a large part of thiol origin still remains unknown. Thus, we only have an incomplete picture of thiol precursors and there is a lack of knowledge on pre-fermentative mechanisms that can impact their levels. Our study focused on the formal identification and the quantification of new varietal thiol precursors in must. First of all, we synthesized natural and labeled standards using an original multi-step strategy, then we developed and validated a UPLC-MS/MS method that allowed us to identify and quantify for the first time a dipeptide S -conjugate to 3MH, the γGluCys-3MH, in Sauvignon B. We observed the S -4-mercapto-4-methylpentan-2-one- l -cysteinyl-glycine (CysGly-4MMP) and S -4-mercapto-4-methylpentan-2-one-N-( l -γ-glutamyl)- l -cysteine (γGluCys-4MMP) but at too low concentration to be quantified. [ABSTRACT FROM AUTHOR]

The inhibitory profiles of chilli pepper and capsaicin, as well as their relationship to the formation of heterocyclic amines (HAs) in roast beef patties were investigated using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with principal component analysis (PCA). HAs including 2-amino-1-methyl-6-phenylimidazo[4,5- b ]pyridine (PhIP), 2-amino-1,6-dimethylimidazo[4,5- b ]pyridine (DMIP), 2-amino-1,5,6-trimethylimidazo[4,5- b ]pyridine (1,5,6-TMIP), 2-amino-3-methyl-3H-imidazo[4,5- f ]quinoxaline (IQx), 2-amino-3,8-dimethylimidazo[4,5- f ]quinoxaline (MeIQx), 2-amino-3,4,8-trimethyl-3H-imidazo[4,5- f ]quinoxaline (4,8-DiMeIQx), 1-methyl-9H-pyrido[3,4- b ]indole (harman) and 9H-pyrido[3,4- b ]indole (norharman) were detected and quantified in beef patties. Different levels of chilli pepper and capsaicin had different inhibitory profiles on HA formation, but had no significant (P > 0.05) effect on the texture of the patties. Furthermore, all levels of chilli pepper and capsaicin reduced total HA and PhIP concentrations dose-dependently, with the highest inhibitions of 80% and 98% at 2 mg of capsaicin. Moreover, capsaicin inhibited all HAs more than chilli pepper, implying that ingredients other than capsaicin in chilli pepper may promote the formation of HAs. These results could be useful for the reduction of HA, during food processing procedures, by spices [ABSTRACT FROM AUTHOR]

An effective analytical method was developed for the detection and quantification of polyoxin D in butterbur using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were extracted using acidified deionised water and purified via solid-phase extraction (SPE) using an HLB cartridge. An external matrix-matched standard calibration curve was prepared, which provided an excellent linearity with a coefficient of determination ( R 2 ) ⩾0.999. Limits of detection (LOD) and quantification (LOQ) were 0.015 and 0.0.05 μg/g, respectively. The developed method was validated in terms of recovery performance using two fortification levels in triplicate. The storage stabilities of the various field samples were also determined. Our method provided consistent recovery (86.26–87.37%) with a relative standard deviation (RSD) of <5%, and was successfully applied to field-treated butterbur grown under greenhouse conditions and collected at various times following commercial fungicide application. As expected, a gradual degradation of polyoxin D was observed, with a half-life (t 1/2 ) of 2.11 d being recorded. Finally, we propose that the developed method can be extrapolated to other crops for routine analysis and can be used to determine the pre-harvest intervals (PHIs), thus preventing the development of antibiotic resistance genes in humans and in the environment. [ABSTRACT FROM AUTHOR]

• QuEChERS based simultaneous extraction method was developed for PAHs and HAs. • A high recovery of HAs by UPLC-MS/MS and PAHs by GC–MS/MS was shown. • Roasting pork jerky at 220 °C generated more PAHs than at 180 °C, but unaffected HAs. • Sugar addition reduced HAs & PAHs during roasting and soy sauce reduced some PAHs. • Addition of 0.5% curcuma/cinnamon powder inhibited HAs formation, but not PAHs. Heterocyclic amines (HAs) and polycyclic aromatic hydrocarbons (PAHs) are widely distributed in foods. This study aims to extract PAHs and HAs from pork jerky simultaneously by QuEChERS for analysis by GC–MS/MS and UPLC-MS/MS, respectively. Also, the effects of flavoring materials and processing temperature on the formation of PAHs and HAs were studied. Acetonitrile containing 1% acetic acid possessed the highest extraction efficiency, with high accuracy and precision being attained for HAs and PAHs. Pork jerky roasted at 220℃ generated a higher PAHs content than 180℃, but unaffected the HAs formation. Addition of sugar reduced formation of both HAs and PAHs during roasting, while soy sauce reduced some PAHs and promoted HAs formation. Incorporation of 0.5% curcuma or cinnamon powder inhibited HA formation with a more pronounced effect being shown by the latter, but neither inhibited PAH formation. The correlation between HA and PAH formation was assessed by principle component analysis. [ABSTRACT FROM AUTHOR]

This study describes the optimization and single-laboratory validation of a single residue method for determination of two bipyridylium herbicides, paraquat and diquat, in cowpeas by UPLC-MS/MS in a total run time of 9.3 min. The method is based on extraction with an acidified methanol-water mixture. Different extraction parameters (extraction solvent composition, temperature, sample extract filtration, and pre-treatment of the laboratory sample) were evaluated in order to optimize the extraction method efficiency. Isotopically labeled internal standards, Paraquat-D6 and Diquat-D4, were used and added to the test portions prior to extraction. The method validation was performed by analyzing spiked samples at three concentrations (10, 20 and 50 μg kg −1 ), with seven replicates (n = 7) for each concentration. Linearity (r 2 ) of analytical curves, accuracy (trueness as recovery % and precision as RSD%), instrument and method limits of detection and quantification (LOD and LOQ) and matrix effects were determined. Average recoveries obtained for diquat were between 77 and 85% with RSD values ⩽20%, for all spike levels studied. On the other hand, paraquat showed average recoveries between 68 and 103% with RSDs in the range 14.4–25.4%. The method LOQ was 10 and 20 μg kg −1 for diquat and paraquat, respectively. The matrix effect was significant for both pesticides. Consequently, matrix-matched calibration standards and using isotopically labeled (IL) analogues as internal standards for the target analytes are required for application in routine analysis. The validated method was successfully applied for cowpea samples obtained from various field studies. [ABSTRACT FROM AUTHOR]

This paper reports on the environmental rhodamine B (RhB) contamination in capsicum caused by agricultural materials during the vegetation process. Ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was applied to detect 64 capsicum samples from China, Peru, India and Burma. Results demonstrated that RhB was found in all samples at low concentrations (0.11–0.98 μg/kg), indicating RhB contamination in capsicums is probably a ubiquitous phenomenon. In addition, studies into soils, roots, stems and leaves in Handan of Hebei province, China showed that the whole ecologic chain had been contaminated with RhB with the highest levels in leaves. The investigation into the agricultural environment in Handan of Hebei province and Korla of Xinjiang province, China demonstrated that the appearances of RhB contamination in the tested capsicums are mainly due to the agricultural materials contamination. The study verified that environmental contamination should be an important origin for the RhB contamination in capsicum fruits. [ABSTRACT FROM AUTHOR]

We hereby report the transformation of deoxynivalenol (DON) and its acetylated derivatives (3-ADON and 15-ADON) by spiking targeted mycotoxins to Fusarium mycotoxin-free flour in the process of making Chinese steamed bread (CSB). The impacts of pH, yeast level, and steaming time on the transformation of 3-ADON to DON were investigated. DON, 3-ADON, and 15-ADON were analyzed by UPLC–MS/MS. Spiked DON was stable throughout the CSB making process. Spiked 3-ADON and 15-ADON were partially deacetylated and transformed to DON during kneading (54.1–60.0% and 59.3–77.5%, respectively), fermentation (64.0–76.9% and 78.2–91.6%, respectively), and steaming (47.2–52.7% and 52.4–61.9%, respectively). The ADONs level increased after steaming compared with their level in the previous step. The pH level and steaming duration significantly ( P < 0.05) affected the conversion of 3-ADON during the CSB making process. Briefly, alkaline conditions and short steaming times favored the deacetylation of 3-ADON. The level of yeast did not remarkably ( P < 0.05) alter the transformation between ADONs and DON. [ABSTRACT FROM AUTHOR]

Organophosphate esters (OPEs) are common flame retardants that are used in a wide variety of products. These compounds might migrate into and pollute food products. An analytical method involving an improved approach called the “quick, easy, cheap, effective, rugged, and safe” (QuEChERS) method and ultra-performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS) was developed to simultaneously measure trace levels of nine OPEs in milk powder. Separation of the nine OPEs was optimized on a reversed-phase column within 7 min. The stable isotope tri-n-butyl phosphate- d 27 (TBP- d 27 ) was used as an internal standard. This method was validated in terms of its linearity, sensitivity, precision, accuracy and matrix effects. Matrix-matched calibration curves were constructed with 1/ x 2 as the weighting factor for all of the target compounds resulting in coefficients of regression lines between 0.9938 and 0.9999. The average accuracy was between 73.5% and 110.2%. Intra- and inter-assay precisions for six replicates ranged from 3.9% to 8.9% or below 11%, respectively. The limits of detection (LODs) were in the range of 0.1–0.25 μg/kg, and the limits of quantification (LOQs) were below 1.5 μg/kg. Significant matrix effects have been observed, but suppression or enhancement of the signal was compensated for by the use of an isotopically labeled internal standard. This validated method was successfully applied to determine the concentrations of the OPEs in milk powder. [ABSTRACT FROM AUTHOR]

• A satisfactory recovery of flavonoids was obtained by UA-ATPE after RSM optimization. • Rutin, quercetin 3-β- d -glucoside, kaempferol 3-rutinoside composed flavonoids in JPs. • Multiple forces promoted the mass transfer of solvent to cells of JPs. • JPs flavonoids were captured by W/W emulsion in bottom phase and distributed to top. The ultrasound-assisted aqueous two-phase extraction (UA-ATPE) was employed to develop an effective technique for the extraction of flavonoids from jujube peels (JPs). The extraction conditions were further optimized as K 2 HPO 4 35% (w/w), ethanol 20% (w/w), solid–liquid ratio 1:30 g/mL (w/v), ultrasonic power 200 W, and extraction time 50 min. Moreover, rutin, quercetin 3-β- d -glucoside, and kaempferol-3-O-rutinosid were identified as the main flavonoids by UPLC-MS/MS. Finally, the extraction mechanism of UA-ATPE was explored, which is salting out effect, hydrogen bonding, van der Waals force, and ultrasound promoted the mass transfer of solvent to cells of JPs, then extraction behavior occurred. The mechanical destruction of JPs cells by ultrasound also further accelerated the release of flavonoids. Flavonoids were captured by W/W emulsion in the bottom phase and distributed to the top phase. Overall, this study proposes a green and clean method, UA-ATPE, to extract flavonoids from JPs, while revealing the mechanism of UA-ATPE. [ABSTRACT FROM AUTHOR]

The present study investigated the changes and conversion profiles of DON, its conjugations 3-ADON, and 15-ADON during bread making process, by spiking targeted mycotoxin standards to Fusarium mycotoxins-free wheat flour. No significant ( p < 0.05) changes of DON levels were observed during dough preparation stages, including kneading, fermentation, and proofing. A reduction of DON level ranged from 4% to 14% was observed during baking process. The main thermal degradation products of DON, namely norDON A, B, C, and F were detected in the bread crust. Regarding ADONs, decreases of 20–40% for 3-ADON and 28–60% for 15-ADON were found during fermentation stage, and further losses of ADONs were observed after proofing process. Although ADONs levels gained an increase after baking. This study demonstrated that ADONs were converted to DON, while no ADONs were detectable in DON spiked samples during bread making process. The mechanism that ADONs could be converted into DON is unclear so far. [ABSTRACT FROM AUTHOR]

A selective and rapid method has been developed to determine, simultaneously, 38 veterinary antibiotic residues in raw milk by ultra-high-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS). One milliliter of raw milk was diluted with 0.5 mL water and 3 mL acetonitrile, then purified using an Oasis HLB cartridge. The eluates were evaporated by nitrogen drying and then reconstituted to 4 mL with water/acetonitrile (8:1) before being injected into the UPLC–MS/MS system. The results indicated recoveries of 68–118% for 14 β-lactams, 79–118% for eight quinolones, 71–106% for eight sulfonamides, 76–116% for four tetracyclines, 78–106% for three macrolides, and 88–103% for one lincosamides, with coefficients of variation less than 15% for intraday and interday precisions. The limit of quantification for all antibiotics was 0.03–10 μg kg −1 . This methodology was then applied to field-collected real raw milk samples and trace levels of four antibiotics were detected. [ABSTRACT FROM AUTHOR]

A rapid, effective and sensitive method to quantitatively determine ametoctradin residue in apple, cucumber, cabbage, tomato and grape was developed and validated using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC–MS/MS). The target compound was determined in less than 5.0 min using an electrospray ionisation source in positive mode (ESI+). The limit of detection was below 0.043 μg kg −1 , whereas the limits of quantification did not exceed 0.135 μg kg −1 in all five matrices. The method showed excellent linearity ( R 2 > 0.9969) for the target compound. Recovery studies were performed in all matrices at three spiked levels (1, 10 and 100 μg L −1 ). The mean recoveries from five matrices ranged from 81.81% to 100.1%, with intra-day relative standard deviations (RSDr) in the range of 0.65–7.88% for the test compound. This method will be useful for the quick and routine detection of ametoctradin residues in potato, grape, cucumber, apple and tomato. [ABSTRACT FROM AUTHOR]