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Abstract: Rice herbicide drift poses a significant challenge in California, where rice fields are near almond, pistachio, and walnut orchards. This research was conducted as part of a stewardship program for a newly registered rice herbicide and specifically aimed to compare the onset of foliar symptoms resulting from simulated florpyrauxifen-benzyl drift with residues in almond, pistachio, and walnut leaves at several time points after exposure. Treatments were applied to one side of the canopy of 1- and 2-yr-old trees at 1/100X and 1/33X of the florpyrauxifen-benzyl rice field use rate of 29.4 g ai ha–1 in 2020 and 2021. Symptoms were observed 3 d after treatment (DAT) for pistachio and 7 DAT for almond and walnut, with peak severity at approximately 14 DAT. While almond and walnut symptoms gradually dissipated throughout the growing season, pistachio still had symptoms at leaf out in the following spring. Leaf samples were randomly collected from each tree for residue analysis at 7, 14, and 28 DAT. At 7 DAT with the 1/33X rate, almond, pistachio, and walnut leaves had florpyrauxifen-benzyl at 6.06, 5.95, and 13.12 ng g–1 fresh weight (FW) leaf, respectively. By 28 DAT, all samples from all crops treated with the 1/33X drift rate had florpyrauxifen-benzyl at less than 0.25 ng g–1 FW leaf. At the 1/100X rate, pistachio, almond, and walnut residues were 1.78, 2.31, and 3.58 ng g–1 FW leaf at 7 DAT, respectively. At 28 DAT with the 1/100X rate, pistachio and almond samples had florpyrauxifen-benzyl at 0.1 and 0.04 ng g–1 FW leaf, respectively, but walnut leaves did not have detectable residues. Together, these data suggest that residue analysis from leaf samples collected after severe symptoms may substantially underestimate actual exposure due to the relatively rapid dissipation of florpyrauxifen-benzyl in nut tree foliage.

Proquinazid is a new-generation fungicide authorized in the EU for combating powdery mildew infections in high-value crops. Due to the perishable nature of fruits, alternative analytical methods are necessary to protect consumer's health from pesticide residues. Currently, immunoassays are a well-established approach for rapidly monitoring chemical contaminants. However, the production of high-quality immunoreagents, such as antibodies and bioconjugates, is essential. This study presents a newly designed hapten that maintains the characteristic moieties of proquinazid unmodified. The linear aliphatic substituents of this molecule were used to introduce the spacer arm. A three-step synthesis strategy was optimized to prepare a hapten that displays the entire 6-iodoquinazolin-4(3H)-one moiety with excellent yields. The N-hydroxysuccimidyl ester of the hapten was activated and purified to prepare a protein conjugate with high hapten density, which was used as an immunogen. Antibodies were raised and competitive enzyme-linked immunosorbent assays were developed. To enhance the assay's sensitivity, two additional heterologous haptens were prepared by modifying the halogenated substituent at C-6. The optimized assays demonstrated low limits of detection in buffer, approximately 0.05 μg/L. When applied to the analysis of proquinazid in QuEChERS extracts of strawberry samples, the immunoassays produced precise and accurate results, particularly in the 10–1000 μg/kg range. [ABSTRACT FROM AUTHOR]

Fiber technology, crucial to human societies for millennia, encompasses cordage and textiles. The development of fiber crops and the production of fiber-based clothing are significant components of the Neolithic Revolution. Despite China being an independent center for agriculture, the role of fiber technology in this context remains largely unexplored. In this project, we employed a comprehensive approach that combines microfossil analysis and use-wear examinations to study tools from the Peiligang site in North China. This site uniquely spans the Upper Paleolithic and early Neolithic periods, offering an ideal setting for investigating the evolution of fiber production. Our results reveal that some Paleolithic blades and scrapers were associated with fiber production, which coincided with ostrich eggshell beads and hematite during the cold and dry Last Glacial Maximum period. Responding to climatic fluctuations, fiber production played a significant role in subsistence and ritual activities. In the early Neolithic, advanced fiber production is evident. Two adjacent burials yield tools and microfossil remains representing a toolkit for fiber and possible textile production, including harvesting, retting, pounding, scraping, and sewing. Fibers recovered from human bones provide potential evidence of textile production and use. Dyeing with blue, black, and red colorants was common for textiles, cordages, and strings. These grave goods suggest the involvement of the deceased in craft production with bast fibers, possibly embodying the earliest specialization in fiber craft 8000 years ago in Neolithic China. [ABSTRACT FROM AUTHOR]

The residue issues resulting from improper use of pesticides occurs frequently in animal origin foods, and its potential risks to human health have drawn attention gradually. This study developed a method based on ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the simultaneous detection of clethodim and its metabolites, clethodim sulfone and clethodim sulfoxide, in pork, chicken liver, and milk samples. The samples were extracted with acetonitrile, followed by liquid-liquid partitioning with n-hexane and purification with C18 solid-phase dispersion. The results showed that clethodim and its metabolites exhibited good linearity in pork, chicken liver, and milk (R² ≥ 0.9956), with limits of quantification (LOQ) of 0.01, 0.01, and 0.005 mg/L, respectively. The recovery of the method ranged from 84% to 108%, with relative standard deviations (RSD) between 1% and 10%. Compared with other reported methods, the developed method reduced the consumption of organic solvent and achieved higher sensitivity. The established method was used to detect 90 samples of pork, chicken liver, and milk that collected from supermarkets across the country, and no residues of clethodim or its metabolites, clethodim sulfone and clethodim sulfoxide, were detected. The results provide reference for the establishment of standard detection methods for clethodim and its metabolites in animal-derived samples in China. [ABSTRACT FROM AUTHOR]

Fireworks play a vital role in festive celebrations and entertainment. These fireworks industries are administered by the Petroleum and Explosives Safety Organisation (PESO), Nagpur, Government of India. Even though PESO prescribed the standard composition for various fireworks products, concerns persist regarding the potential deviation from these standards, particularly in the pursuit of increased noise levels to attract consumers. This change in the burning and reactive properties of chemicals could potentially lead to accidents and environmental pollution. The current work investigated the combustion characteristics of two unknown market flash powder samples and a PESO standard sample. The samples were openly ignited in a controlled atmosphere, and video recordings of the resulting chemical flames were analyzed to determine fire area, flame intensity, and motion magnitude. The residues were also collected for EDAX and SEM analysis. Fire pixels from video frames are segmented to create a comprehensive database detailing flame area and motion magnitude under different circumstances. From the flame area profile, motion magnitude and SEM/EDAX analysis, it is found that PESO standard sample combustion is better than the unknown flash powder combustion. • Burning flame of fireworks chemicals captured by CCD. • Flame area and volume had been found by Digital Image Processing. • Residue analysis was carried out. • Through flame analysis and residue analysis, fuel properties had been explored. [ABSTRACT FROM AUTHOR]

Copyright of Journal of Food Safety & Quality is the property of Journal of Food Safety & Quality Editorial Department and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Copyright of Food & Fermentation Industries is the property of Food & Fermentation Industries and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Copyright of Journal of Food Safety & Quality is the property of Journal of Food Safety & Quality Editorial Department and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

A simple, sensitive, and rapid spectrophotometric method for the determination of Cu(II), Ni(II), Co(II), and Mn(II) ions is proposed based on the complexation of metal ions with a synthesized ligand, 4-methylpiperazine dithiocarbamic acid, formed by the reaction of 4-methyl piperazine and carbon disulfide under cold conditions. The colored complex formed by the reaction of the synthesized ligand with these heavy metals in an aqueous acetonitrile medium exhibits absorbance maxima at 435, 395, 370, and 495 nm for Cu, Ni, Co, and Mn metals, respectively. Beer's law was valid within concentration ranges of 0.34–20.46, 0.49–39.81, 0.47–38.07, and 0.49–11.03 µg/mL for Cu, Ni, Co, and Mn, respectively. Various reaction parameters such as pH, volume of reagent, and solvents were carefully studied and optimized. The limits of detection and limits of quantification for Cu, Ni, Co, and Mn were found to be 1.4, 2.4, 1.1, and 1.1 µg/mL and 4.2, 7.2, 3.3, and 3.3 µg/mL, respectively. The method proved to be sensitive and rapid, requiring only a few minutes for sample analysis. The synthesized ligand and metal(II) 4-methyl piperazine dithiocarbamate complexes, M(4-methylPzdtc)2, were characterized by FTIR. The method was subsequently applied to vegetable and water samples spiked with the cations. The high recoveries of Cu, Ni, Co, and Mn from the proposed method indicate good accuracy and precision. [ABSTRACT FROM AUTHOR]

The search is on for safer alternatives to fumigants like methyl bromide and phosphine, which harm the ozone layer and pose other risks. Ethyl formate is a promising candidate due to its potential antimicrobial and insecticidal action in stored products like date fruits. The susceptibility of date fruits to microbial spoilage is significantly influenced by factors such as moisture content, storage practices, and environmental conditions. In the present study, the in vitro antimicrobial effect of ethyl formate against three microbial species, namely Aspergillus niger F4, Mucor circinelloides YMM22, and Pseudomonas aeruginosa B1 was tested under laboratory conditions. In addition, two common date fruit varieties, semi-dry El-Wady I and the dry Frehi, were fumigated with ethyl formate alone in a laboratory-scale prototype and with a mixture of ethyl formate and CO2 at a semi-industrial scale prototype. Both varieties had an initial moisture content of around 13.40 and 12.48% for El-Wady I and Frehi, respectively. The fumigation was conducted using the optimal concentration of 70 mg/L air for 24 h incubation period. Fumigation with ethyl formate alone or in combination with CO2 significantly reduced the number of viable bacteria and fungi (CFU/g), but the potential for a combined effect with CO2 was not investigated. The percentages of reduction in the fungal count were 78.18 and 90.76% for Frehi and El-Wady I varieties, respectively in a semi-industrial scale prototype. Moreover, the percentages of reduction in the bacterial count were 53.31 and 65.20%, respectively for Frehi and El-Wady I varieties. Ethyl formate showed promise as a natural alternative to control microbial contamination of stored date fruits. Further research suggests that increasing fumigation duration or concentration could provide comprehensive control of microbial pathogens at all stages of development. [ABSTRACT FROM AUTHOR]

The widespread use of fenobucarb and propoxur insecticides for agricultural and non-agricultural purposes causes undesirable effects on human health and environment due to their residues in surface and ground water resources. In view of this, two new, simple, accurate, sensitive, economical and reproducible optical methods have been investigated for the determination of fenobucarb and propoxur insecticides in pure form, in their commercial formulations, and agricultural samples viz. water, grains and vegetables. The methods are based on the alkaline hydrolysis of the insecticides to methyl amine and the reaction of the latter to give colored products. In the spectrophotometric method, the methyl amine formed, in presence of carbon disulfide (CS2) and Ni(II) acetate gives a yellow colored complex, which was measured at 370 nm. Beer's law is valid in the concentration range of 0.41–8.29 and 0.42–8.37 µg mL−1 for fenobucarb and propoxur, respectively. The spectrofluorimetric method is based on the study of yellow-colored product, formed by the condensation of methyl amine with acetylacetone and formaldehyde (Hantzsch reaction), at pH 5.5. The reaction product exhibits fluorescence intensity at an emission wavelength of 470 nm after excitation at a wavelength of 390 nm for both fenobucarb and propoxur insecticides. The method has linearity range of 0.14–5.53 and 0.14–5.58 µg mL−1 for fenobucarb and propoxur, respectively. The different factors which affect the reactions were thoroughly studied and optimized. The proposed methods have been successfully applied to assay both insecticides in their commercial formulations and for recovery study from spiked environmental samples. The good results of recoveries of both insecticides demonstrate the accuracy and precision of both methods. [ABSTRACT FROM AUTHOR]

Chiral pesticides have one or more enantiomers, and their biological activity, toxicity, environmental behavior, degradation and metabolism may be different. Tea, as one of the three major beverages, has attracted much attention in terms of quality and safety. However, more attention is currently paid to the total amount of pesticide racemate residues. With the development of analytical techniques, it is particularly crucial to fully understand the stereoselective behavior of the chiral pesticide enantiomer in tea, as well as to examine residue degradation in tea and to set the maximum residue limits for enantiomers. This would help to improve the efficacies of chiral pesticides and reduce their residues and toxicities to non-target organisms. In this paper, the current status of chiral pesticide separation and residue detection technology in tea were reviewed, such as liquid chromatography, gas chromatography and supercritical fluid chromatography. In addition, it provided a summary of the residue degradation behaviors and risk assessment of chiral pesticide enantiomers in tea, which would be useful as a guide for further in-depth studies on chiral pesticide enantiomers in tea. [ABSTRACT FROM AUTHOR]

In this study, the separation conditions of UHPLC-QTOF-MS and the extraction conditions of QuEChERS were optimized. The analytical process for determining Broflanilide residues in different soil types was successfully established and applied to its adsorption, desorption, and leaching in soil. Broflanilide was extracted from soil with acetonitrile and purified using PSA and MgSO4. The modified UHPLC-QTOF-MS method was used for quantification. The average recovery of Broflanilide was between 87.7% and 94.38%, with the RSD lower than 7.6%. In the analysis of adsorption, desorption, and leaching quantities in four soil types, the RSD was less than 9.2%, showing good stability of the method, which can be applied to determine the residue of Broflanilide in different soils. [ABSTRACT FROM AUTHOR]

The paper presents the results of an interim analytical approach to the Late Roman shipwreck of Ses Fontanelles recently found in the island of Mallorca (Balearic Islands, Spain). The excellent state of preservation of the hull and the cargo, including amphorae with painted inscriptions (tituli picti), and its location in shallow waters offshore of one of the main touristic beaches of the island makes this a unique finding in the Mediterranean. A first season of excavations and study of the cargo triggered an analytical approach to solve some of the problems pose by archaeological research, mainly related to the possible origin of the vessel. The analytical strategy combines petrographic analysis for the study of the provenance of the amphorae, archaeozoology and residue analysis to identify their content, and analysis of the wood and plant remains to understand the use of vegetal resources in shipbuilding and in the stow of the cargo. The results of the combination of the petrographic analysis, the study of the ichthyofauna and the organic residue analysis suggest that the boat probably departed from the area of Cartagena in the southeastern part of the Iberian Peninsula, carrying a cargo of fish sauce (liquaminis flos), oil, and wine (probably also some olives preserved in grape derivatives), transported in three main types of amphorae. The analysis of the wood shows, as known in Roman shipbuilding, a clear selection of forest resources. The shipbuilders used pine for longitudinal parts of the hull, while for the small pieces related to the assemblage system (pegged, mortise and tenons) and subjected to a great stress they selected harder woods mainly Cupressaceae, Olea europaea, and Laurus nobilis. In addition, the study reveals that mainly branches of Vitis vinifera, but also other herbaceous plants were used as dunnage protecting the cargo during the journey. The results help to shed some light into different aspects of this unique vessel sunk in Mallorcan waters and contributes to show the benefit of applying archaeological sciences in maritime archaeology. [ABSTRACT FROM AUTHOR]

This work presented an analytical method to determine hainanmycin in chicken meat and eggs using ultra high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The extraction was carried out using a modified QuEChERS procedure followed by a cleanup combination of OASIS HLB SPE and freezing lipid filtration. The analyte was determined by UHPLC-MS/MS in positive ESI mode using ammonia adduct [M + NH4]+ as the precursor ion. The method was comprehensively validated according to CIR (EU) 2021/808 and EURL Guidance Document on Confirmation Method Validation. The performance characteristics were linearity, decision limit (CCα), recovery, repeatability, within-laboratory reproducibility, matrix effect, selectivity, ruggedness, and stability. Good linearity was obtained in the 0.05–10 μg/L concentration range with coefficient of determination (R2) higher than 0.99. The CCα values ranged from 0.21 to 0.24 μg/kg; the average recoveries were 80.9–85.5%; and the repeatability and within-laboratory reproducibility were less than 10%. The validation results fulfilled the requirements of EU guidelines. Briefly, the proposed method achieved high sensitivity and accuracy, suitable for determining hainanmycin residue in chicken meat and eggs. [ABSTRACT FROM AUTHOR]

For non-target residue analysis of xenoestrogens in food, sophisticated chromatographic–mass spectrometric techniques lack in biological effect detection. Various in vitro assays providing sum values encounter problems when opposing signals are present in a complex sample. Due to physicochemical signal reduction, cytotoxic or antagonistic effect responses, the resulting sum value is falsified. Instead, the demonstrated non-target estrogenic screening with an integrated planar chromatographic separation differentiated opposing signals, detected and prioritized important estrogenic compounds, and directly assigned tentatively the responsible compounds. Sixty pesticides were investigated, ten of which showed estrogenic effects. Exemplarily, half-maximal effective concentrations and 17β-estradiol equivalents were determined. Estrogenic pesticide responses were confirmed in six tested plant protection products. In food, such as tomato, grape, and wine, several compounds with an estrogenic effect were detected. It showed that rinsing with water was not sufficient to remove selected residues and illustrated that, though not usually performed for tomatoes, peeling would be more appropriate. Though not in the focus, reaction or breakdown products that are estrogenic were detected, underlining the great potential of non-target planar chromatographic bioassay screening for food safety and food control. [ABSTRACT FROM AUTHOR]

Sulfolane, a highly water-soluble industrial solvent, has raised environmental concerns due to its widespread usage and its prolonged persistence once released into the environment. To assess the extent of contamination effectively, reliable analytical methods are essential. In this review article, the existing methodologies for the sample preparation and determination of sulfolane are systematically examined and evaluated. In brief, existing guidelines for sampling from environmental matrices provide a solid foundation for sulfolane analysis. Notably, there is little variation in the choice of final determination methods, with GC-MS or GC-FID being favored across all studies. However, substantial variability emerges in sample preparation methods. Moreover, upon scrutiny of the analytical procedures utilized in sulfolane analysis, it becomes evident that a considerable number of them are characterized by inefficiency or environmental hazards, often relying on substantial quantities of chlorinated solvents. Through this review, valuable insights into the challenges at hand and potential solutions can be gained, offering a foundation for the development of novel sulfolane analysis methods applicable to a range of environmental matrices. Overall, this field calls for further research to devise efficient and environmentally sustainable analytical methods for sulfolane analysis. [ABSTRACT FROM AUTHOR]

Migration is a frequent phenomenon in human history. Previous studies mainly used migration as a simple process to account for any cultural changes observed in migrant communities. Recent studies, however, have recognized that migration is embedded in both environmental and social contexts, thus making it necessary to study the consequence of migration on a case-by-case basis. To better understand the changes associated with migrational processes, this case study investigates the subsistence pattern of a Neolithic site (5300-4700 cal. BP), Liujiazhai, in Northwestern Sichuan Highland by employing microbotanical residue analysis on pottery vessels. Our results on millet phytolith contribute to the overall picture of millet agriculture in Yangshao and Majiayao migrant communities and enrich our understanding of how varying crop patterns in Neolithic western China are likely a consequence of migration. In addition, we suggest that Liujiazhai migrants adapted to the high-altitude environment by utilizing more local wild plant resources. This study shows that, although Yangshao migrants were still connected to their homeland in terms of material culture, relocating to the challenging environment in NW Sichuan requires adaptive strategies that diverged the Yangshao migrants, including Liujiazhai, from their home culture. Hence, this study exemplifies how migration is an agent of change. [ABSTRACT FROM AUTHOR]

Objective: This study aimed to establish a method for the Preparation of matrix reference material for carbaryl residues in Chinese yam flour. Methods: Yam powder containing menafyl was prepared by homogenized, freeze-dried, ground, sifted, mixed and packaged. A liquid chromatography-series mass spectrometer was used for detection, and the isotope internal standard curve method was used for quantification. Through the process of equalization stability evaluation, cooperative setting and uncertainty evaluation, the matrix reference material of the expected yam powder was obtained. Results: The property value and expanded uncertainty of carbaryl was (1.04±0.10) mg/kg (k=2). Conclusion: It could be used for food laboratory method verification, quality control and other activities.

Abstract Background Ethyl formate (EF) is naturally occurring volatile compound used as quarantine fumigant for pest control. Recently, conversion of uses of EF was tried from quarantine to agricultural field due to its promising efficacy. However, there is a lack of studies on the residue pattern on crops and soil and the phytotoxic mechanism of EF in greenhouse environment. This study aimed to evaluate the efficacy, residue analysis, and phytotoxicity of EF fumigation in controlling Myzus persicae and Thrips palmi, on cucurbit crops and establish an optimized fumigation strategy for use in greenhouses. Results The results showed that EF was more effective against M. persicae than against T. palmi. Residue analysis indicated that EF rapidly decomposed and was not retained after 30 min in leaves and 2 h in soil after fumigation, suggesting the potential for residue-free pest control. Phytotoxicity test revealed that watermelon was the most sensitive crop to EF, and H2O2 accumulation was observed above a concentration of 7.5 g/m3. A strategy to reduce phytotoxicity with sodium bicarbonate during fumigation showed promising results in reducing phytotoxic effects on the crops. The optimized EF fumigation with 6 g/m3 was applied in a greenhouse, resulting in 100% and 40% mortality of M. persicae and T. palmi, respectively, with no notable phytotoxicity and EF residue in the treated crops and soil. Conclusion This study demonstrates that optimized EF fumigation can be an environmentally sustainable method for controlling pests in greenhouses, paving the way for improved pest management practices and sustainable agriculture. Further research is needed to validate these findings and explore the potential of EF fumigation for other crops and pests. Graphical Abstract

Tel Megiddo is a major type‐site for the Middle Bronze in the Levant. During this period a new burial custom appeared in which the dead were interred beneath occupied houses. This tradition is well attested in Area K at the site. Area H, near the palatial complex, revealed a monumental masonry‐constructed chamber tomb. This article presents the results of residue analysis conducted on ceramic vessels placed in these tombs as burial offerings. Hundreds of intramural Middle Bronze tombs with ceramic offerings were excavated in the Levant, but this is the first time the content of the vessels is revealed. [ABSTRACT FROM AUTHOR]

With frequent RASFF notifications from the EU countries, the residue testing of ethylene oxide (EtO) and its metabolite 2-chloroethanol (2-CE) in food commodities has become essential to check their compliance with MRLs. This study, for the first time, aimed at establishing a dynamic headspace-GC-MS/MS method for the simultaneous determination of these two analytes in acetonitrile extracts of cumin, ashwagandha, chilli powder, turmeric powder, guar gum, locust bean gum, and ginger powder. The samples (4 g) were extracted using acetonitrile (10 mL). A dispersive-solid phase extraction cleanup step with primary secondary amine sorbent (50 mg/mL) reduced the interfering signal of (matrix-derived) acetaldehyde by >40% in chilli powder, ginger, turmeric, and guar gum. This cleanup was not required for sesame seeds. With high selectivity and sensitivity, the GC-MS/MS approach identified and quantified both compounds simultaneously. At the spiking levels of 0.01, 0.02, and 0.05 mg/kg, the recoveries and precision were satisfactory (70–120%, RSDs, ≤15%). The headspace method-performance was similar to liquid injections. The method provided reproducible results when evaluated by two different laboratories. The method provided high-precision results for incurred residue analysis. Given its efficiency, the validated method is anticipated to improve the effectiveness of monitoring of EtO residues in food commodities. [ABSTRACT FROM AUTHOR]

The excessive use of glufosinate˗ammonium herbicide and carbofuran insecticide in agriculture leaves residues on agricultural samples and contaminates groundwater and surface water bodies through surface runoff and through leaching. To monitor pollution from the use of these pesticides, two simple, accurate and precise optical methods for their determination have been developed and validated in the commercial formulation and agricultural samples, viz., water, grains and vegetables. The first method is based on the reaction of the amino function of both pesticides with carbon disulfide and Ni(II) acetate in an aqueous acetonitrile medium and the measurement of color developed at 380 and 365 nm for glufosinate˗ammonium and carbofuran, respectively. Beer's law was valid within a concentration range of 0.4–8 and 0.4–9 µg/mL for glufosinate˗ammonium and carbofuran, respectively. The second spectrofluorimetric method is based on the condensation of the primary amino group of glufosinate˗ammonium and carbofuran with acetylacetone and formaldehyde (Hantzsch reaction) in the presence of buffer of pH 5.5 producing a yellow˗colored product. The fluorescence intensity of the reaction products was measured at an emission wavelength of 470 nm after excitation at a wavelength of 380 nm for glufosinate-ammonium and 388 nm for carbofuran. The linearity range found was 0.13–5 and 0.14–6 µg/ mL for glufosinate˗ammonium and carbofuran respectively. All the variables affecting the reactions, such as hydrolysis time, heating time, pH, concentration and volume of reagent were carefully studied and optimized. The high recoveries of glufosinate-ammonium and carbofuran from spiked water, grain and vegetable samples in both methods indicate good accuracy and precision of the methods. [ABSTRACT FROM AUTHOR]

For 15 years, the University of Idaho has conducted chemical testing of excavated materials from historical sites throughout North America. The most common artifacts tested are sealed containers. Some come from current excavations, but most are from repository shelves. The immediate purpose of the archaeochemistry work is twofold: to identify the contents of the containers for researchers and to provide training for students in analytical chemistry. After testing more than 500 items, project personnel have recognized some unexpected outcomes that have implications for institutions housing the artifacts. Specifically, tested materials identified the small, yet consistent, presence of certain artifacts that can have health implications for personnel working with the items. The article concludes with general guidance on identifying and assessing those risks. [ABSTRACT FROM AUTHOR]

Background: Ethyl formate (EF) is naturally occurring volatile compound used as quarantine fumigant for pest control. Recently, conversion of uses of EF was tried from quarantine to agricultural field due to its promising efficacy. However, there is a lack of studies on the residue pattern on crops and soil and the phytotoxic mechanism of EF in greenhouse environment. This study aimed to evaluate the efficacy, residue analysis, and phytotoxicity of EF fumigation in controlling Myzus persicae and Thrips palmi, on cucurbit crops and establish an optimized fumigation strategy for use in greenhouses. Results: The results showed that EF was more effective against M. persicae than against T. palmi. Residue analysis indicated that EF rapidly decomposed and was not retained after 30 min in leaves and 2 h in soil after fumigation, suggesting the potential for residue-free pest control. Phytotoxicity test revealed that watermelon was the most sensitive crop to EF, and H2O2 accumulation was observed above a concentration of 7.5 g/m3. A strategy to reduce phytotoxicity with sodium bicarbonate during fumigation showed promising results in reducing phytotoxic effects on the crops. The optimized EF fumigation with 6 g/m3 was applied in a greenhouse, resulting in 100% and 40% mortality of M. persicae and T. palmi, respectively, with no notable phytotoxicity and EF residue in the treated crops and soil. Conclusion: This study demonstrates that optimized EF fumigation can be an environmentally sustainable method for controlling pests in greenhouses, paving the way for improved pest management practices and sustainable agriculture. Further research is needed to validate these findings and explore the potential of EF fumigation for other crops and pests. [ABSTRACT FROM AUTHOR]

This paper considers the structure investigated at the largest area (labeled as BII-21B) in the Chalcolithic level BII of Tell Yunatsite, located in the western parts of the Upper Thracian Plain. It collapsed during a sudden fire, which did not affect the neighboring house to the west. The debris sealed a large number of fragmented vessels, plant remains, and even some of the inhabitants. Detailed analysis of the materials found allows for a reconstruction of diet and storage practices, research on vessels’ function and technology, decoration styles, etc. The plant remains are abundant and demonstrate a diverse species composition. The complex is dominated by lentils, barley, and einkorn wheat. Of particular interest is the evidence on purposeful gathering of grapes for producing a drink, perhaps wine. The investigation of the ceramic assemblage shows that it belongs to a developed – but not final – stage of the Late Copper Age in Upper Thrace. It also provides new information about the contact zone between the Karanovo VI and Krivodol cultures in this area.

Analyte stability is more commonly a confounding factor in analytical chemistry than many analysts recognize. In this study, we assessed the stability of 31 common veterinary drugs in water and final extracts of bovine (milk and kidney/liver) and chicken (muscle and egg) matrices. Two different sample preparation methods were evaluated for one-month storage of the final extracts at typical room, refrigerator, and freezer temperatures. Liquid chromatography – mass spectrometry (LC-MS) by triple quadrupole and high-resolution techniques was used for analysis of the extracts spiked at different relevant concentrations for general regulatory purposes (10–1000 ng/g sample equivalent). Comparison of results between two labs demonstrated that stable drugs (≤20% loss) at all tested conditions consisted of danofloxacin, enrofloxacin, florfenicol, flubendazole, hydroxy-flubendazole, flumequine, flunixin, 5-hydroxy-flunixin, lincomycin, and meloxicam. The tested drugs found to be the most unstable (>20% loss at room temperature within a matter of days) consisted of the β-lactams (ampicillin, cefalexin, cloxacillin, and penicillin G). Curiously, the following antibiotics (mostly macrolides) were apparently more stable in sample extracts than water: emamectin, erythromycin, ivermectin, lasalocid, monensin, tilmicosin, tulathromycin, and tylosin. Those and the other drug analytes (ciprofloxacin, doxycycline, florfenicol amine, 2-amino-flubendazole, oxytetracycline, sulfadiazine, sulfadimethoxine, sulfamethazine, and trimethoprim) were mostly stable for a month in refrigerated extracts, especially at higher concentrations, but not in all cases. In practice, freezer storage of extract solutions was found to be acceptable for at least a month, with a few exceptions. [ABSTRACT FROM AUTHOR]

Sub-synchronous resonance (SSR) is a growing concern in wind turbine generators-based series capacitive compensated networks at low wind speed and peak compensation levels. It is feasible to increase the stability of SSR mode caused by a transmission line's passive series compensation by providing active compensation using a flexible ac transmission system controller cooperating with an auxiliary damping controller. This paper presents preordainment and enhancement of SSR mode in DFIG-based series capacitive compensated line by incorporating an additional damping controller into the static synchronous series compensator (SSSC). The auxiliary damping controller modulates the reactive voltage injected by SSSC into the transmission line by considering the appropriate input control signal, reflecting the SSR instability, and giving the maximum damping to the SSR mode. The optimal input control signal is determined via residue analysis, and the design procedure of the auxiliary damping controller is presented using root locus plots. The root locus plots offer a visual representation of the loci for each mode and preordain eigenvalues for new stability, which aids in the design of the auxiliary damping controller. This feature allows to predetermine the SSR mode eigenvalue while before connecting it with SSSC. Accordingly, it provides a controlled dampening to SSR mode such that the desired damping ratio for SSR mode can be achieved without influencing the stability of other modes. The impact of the designed auxiliary damping controller is examined at high compensation levels and low wind speed. The eigenvalue analysis results show that the preordained eigenvalues found using root locus plots are correct and the proposed approach predominantly enhances the stability of SSR mode. The fast Fourier transform (FFT) analysis and transient simulations are used to show the detuning and dampening of SSR mode. The proposed work is executed using MATLAB/Simulink. [ABSTRACT FROM AUTHOR]

Agrochemicals are indispensable materials in agricultural production, used to control or prevent diseases, insects and weeds, and play important roles in ensuring both food security and food safety. Meanwhile, the negative impacts of modern synthetic pesticides on humans and the environment could not be neglected. Thus, the production, registration, application and monitoring of pesticides should be strictly checked to ensure their commercial product quality and safety to human health as well as to the environment. This review summarizes the analytical chemistry involved in the quality control (QC) analysis for commercial formulation, residue analysis, dietary risk assessment and regulation prospects of pesticides. The main concepts and contents of pesticide analytical chemistry are comprehensively introduced and analyzed. In addition, the requirements and criteria of the relevant guidelines from various organizations are discussed. Finally, the research frontier areas and future trending for the invention of new generation of agrochemicals, registration/enforcement, market monitoring and risk management of pesticides are discussed.

It is well known that many Mesolithic and Early Neolithic sites were uncovered during the past century in the Iron Gates region of the North-Central Balkans. The application of diverse analyses on the bioarchaeological remains and artefacts raised many questions, but also offered new ideas about the Mesolithic–Neolithic transitional period in the Middle and Lower course of the Danube. Communities in the Iron Gates consumed fish and exploited the riverbank in prehistory. The stable isotope analyses are implying that these human groups fed on aquatic resources in some periods more than others. Fish remains were also found in settlements, and based on fish-related imagery on sculpted boulders and other artefacts, the bond between the people, river, and the ecosystem was compelling. The idea of this article is to present the possible ways of fish processing at Lepenski Vir using chipped stone tools. Three integrated methodologies, with high levels of interpretation, were applied: use-wear, residue, and archaeozoological analyses. Use-wear and residue analyses were performed on both archaeological and experimental chipped stone tools. The results are considered together with the traces of butchery observed on archaeological samples of fish bones, creating a more coherent picture of the everyday habits of the Iron Gates populations.

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Modified teeth and jaws have long been recognized as important ceremonial objects during the Middle Woodland period of eastern North America. Direct evidence for the manufacture of the objects is exceedingly rare because they are typically recovered from mortuary contexts or ceremonial caches. Here, we present multiple lines of evidence pointing to the manufacture of modified teeth and jaws at the Moorehead Circle post enclosure within the Fort Ancient Earthworks. The convergence of protein residue, lithic use-wear, and faunal data indicate that bear and likely canid bones were modified by artisans working within the Moorehead Circle. These findings add an important new layer of understanding to our knowledge of these objects, human-animal relations, and craft production in the Middle Woodland. [ABSTRACT FROM AUTHOR]

A modified QuEChERS method coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established for residue analysis of 39 pollutants (34 commonly used multi-class pesticides and 5 metabolites) in medlar matrices (fresh, dried, and medlar juice). Samples were extracted using water with 0.1 % formic acid: acetonitrile (5: 10, v/v). The phase-out salts and five different cleanup sorbents (including N-propyl ethylenediamine (PSA), octadecyl silane bonded silica gel (C18), graphitized carbon black (GCB), Carbon nanofiber (C-Fiber) and MWCNTs) were investigated to improve the purification efficiency. The Box-Behnken Design (BBD) study was employed for an optimal solution of the volume of extraction solvent, phase-out salt, and the purification sorbents for the analytical method. The average recoveries of the target analytes in the three medlar matrices ranged from 70 % to 119 % with relative standard deviations (RSDs) of 1.0 %−19.9 %. Screening of market samples (fresh and dried medlars) collected from the major producing regions in China showed that 15 pesticides and metabolites were detected in the samples at concentrations of 0.01–2.22 mg/kg, and none of which exceeded the maximum residue limits (MRLs) set in China. The results showed that the risk of food safety by consumption of medlar products caused by the use of pesticides was low. The validated method could be used for rapid and accurate screening of multi-class multi-pesticide residues in Medlar for food safety.

In this study, the separation conditions of UHPLC-QTOF-MS and the extraction conditions of QuEChERS were optimized. The analytical process for determining Broflanilide residues in different soil types was successfully established and applied to its adsorption, desorption, and leaching in soil. Broflanilide was extracted from soil with acetonitrile and purified using PSA and MgSO4. The modified UHPLC-QTOF-MS method was used for quantification. The average recovery of Broflanilide was between 87.7% and 94.38%, with the RSD lower than 7.6%. In the analysis of adsorption, desorption, and leaching quantities in four soil types, the RSD was less than 9.2%, showing good stability of the method, which can be applied to determine the residue of Broflanilide in different soils.

Copyright of Estonian Journal of Archaeology is the property of Teaduste Akadeemia Kirjastus and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Copyright of Revista del Museo de Antropología is the property of Museo de Antropologia - IDACOR and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

The residue of coronatine in the paddy field environment, as well as five common fruits and vegetables, was analyzed using the QuEChERS pre-treatment technique combined with HPLC-MS in this experiment. Acetonitrile was used as the extractant, while C 18 and multi-walled carbon nanotubes served as adsorbents for sample extraction and purification. Subsequently, the samples were filtered through a 0.2 μm organic filter membrane before detection on the machine. The limits of detection (LOD) and quantification (LOQ) for coronatine in the paddy field environment and five common fruits and vegetables were determined to be 0.0005–0.0035 mg/kg and 0.0018–0.0118 mg/kg, respectively, exhibiting good linear correlation coefficients (R2≥0.9900) at spiked levels ranging from 0.01 to 1 mg/kg. The average intra-day recoveries ranged from 75.19 % to 107.9 %, with relative standard deviations (RSDs) of 1.24 %-12.66 % at spiked levels of 0.05–0.5 mg/kg. [Display omitted] • Coronatine residues in food detected using HPLC-MS following QuEChERS pretreatment. • Investigation of analytical techniques for detecting coronatine residues in fruits and vegetables. • Study on methods of coronatine residue in paddy field environment. [ABSTRACT FROM AUTHOR]

Spinetoram, a novel insecticide developed by Dow AgroSciences, USA, was the focus of this study. The aim of this study was to establish a methodology for determining the digestion dynamics and final residue concentrations of spinetoram in rice soil, brown rice, rice hulls, and rice plants. This was achieved through the utilization of high-performance liquid chromatography(HPLC) in combination with QuEChERS residue analysis. The results showed that the concentrations and peak areas of spinetoram showed a good linear correlation(R2>0.99) in a certain concentration range, and the LOD and LOQ values ranged from 0.0026 to 0.0066 mg/kg and 0.0103–0.0256 mg/kg, respectively.The average intraday recoveries ranged from 88.34 % to 100.64 % with relative standard deviations ranging from 0.93 % to 6.77 %, while interday recoveries ranged from 89.45 % to 98.34 % with relative standard deviations ranging from 1.32 % to 6.18 %. Dissolution kinetics in paddy soil and rice plants followed one-stage kinetics with half-lives ranging from 6.65 days to 6.92 days and from 3.91 days to 5.49 days respectively. The developed simple and sensitive analytical method facilitates the safe application of spinetoram in rice field environments while minimizing potential environmental risks. [Display omitted] • The improved QuEChERS method based on high performance liquid chromatography (HPLC) was employed for spinetoram. • Spinetoram in soil exhibits low durability and is prone to degradation. • The degradation kinetics of spinetoram in paddy field system follows a first-order kinetic equation. • The recommended spraying dosage does not present a risk to consumers, offering guidance for detecting spinetoram residue. [ABSTRACT FROM AUTHOR]

Sulfolane, a highly water-soluble industrial solvent, has raised environmental concerns due to its widespread usage and its prolonged persistence once released into the environment. To assess the extent of contamination effectively, reliable analytical methods are essential. In this review article, the existing methodologies for the sample preparation and determination of sulfolane are systematically examined and evaluated. In brief, existing guidelines for sampling from environmental matrices provide a solid foundation for sulfolane analysis. Notably, there is little variation in the choice of final determination methods, with GC-MS or GC-FID being favored across all studies. However, substantial variability emerges in sample preparation methods. Moreover, upon scrutiny of the analytical procedures utilized in sulfolane analysis, it becomes evident that a considerable number of them are characterized by inefficiency or environmental hazards, often relying on substantial quantities of chlorinated solvents. Through this review, valuable insights into the challenges at hand and potential solutions can be gained, offering a foundation for the development of novel sulfolane analysis methods applicable to a range of environmental matrices. Overall, this field calls for further research to devise efficient and environmentally sustainable analytical methods for sulfolane analysis.

Quinoxalines (Qx) are chemically synthesized antibacterial drugs with strong antibacterial and growth-promoting effects. Qx is heavily abused by farmers, resulting in large residues in animal-derived foods, which pose a serious threat to human health. Desoxyquinoxalines (DQx), which have the highest residue levels, have been identified as the major toxicant and have become a new generation of residue markers. In this study, we prepared monoclonal antibodies (mAb) based on a new generation metabolite (desoxymequindox, DMEQ) and establish an indirect competitive enzyme-linked immunosorbent assay (ic-ELISA) for the rapid determination of Qx residues in food. The mAb exhibited high sensitivity with half maximal inhibitory concentration (IC50) and a linear range of 2.84 µg/L and 0.8–12.8 µg/L, respectively. Additionally, the cross-reactivity (CR) of the mAb showed that it recognized multiple DQx to varying levels. The limits of detection (LOD), limits of quantification (LOQ), and recoveries for the ic-ELISA assay of pork, swine liver, swine kidney, chicken, and chicken liver were 0.48–0.58 µg/kg, 0.61–0.90 µg/kg, and 73.7–107.8%, respectively, and the coefficients of variation (CV) were less than 11%. The results of the ic-ELISA showed a good correlation with LC–MS/MS in animal-derived foods. This suggests that this analytical method can be used for the rapid screening of QX residues. [ABSTRACT FROM AUTHOR]

Despite an outstanding agent for control of Lepidoptera, the diamide insecticide cyclaniliprole (CYCP) is a suspected carcinogen. In the present study, an analytical method was developed for the determination of CYCP in six fruits and vegetables (apple, grape, peach, bell pepper, lettuce, and tomato) using ultrahigh-performance liquid chromatography coupled with tandem mass spectrometry. Sample preparation was carried out by the acetonitrile-salting-out extraction followed by simple and fast cleanup of disposable pipette extraction tip containing styrene divinyl benzene and/or graphitized carbon black. Satisfactory linearity (r > 0.99) was obtained in the calibration range of 0.001–1 µg mL−1. Matrix effects decreased from −9.9–−17.9% to −1.0–−7.6% after the cleanup. The recoveries of CYCP at three spike levels (0.01, 0.1, and 1 mg kg−1) from different matrices were between 75.7% and 111.5%, with the intra-day (n = 5) and inter-day (n = 15) relative standard deviations lower than 12.1%. The limit of quantification was 0.01 mg kg−1. The developed method provides a good reference for routine monitoring of CYCP in these fruits and vegetables. [ABSTRACT FROM AUTHOR]

Field experiments were conducted to investigate the dissipation and persistence residues of trinexapac acid in paddy crop. The treatments consisted of one control and two different concentrations of Trinexapac-ethyl 25% EC (Emulsifiable concentrate) at 30 and 60 g a.i. ha - 1 (recommended and double the recommended dose). Leaf samples were collected at random in each plot separately at 0, 1, 3, 5, 7, 10 and 15 days after foliar application and grain, straw and soil samples were collected at harvest. The mean recovery of trinexapac acid (@ 0.01, 0.05 and 0.1 mg kg - 1 was more than 75%. At application rate of 30 and 60 g a.i. ha - 1 (gram of active ingredient per hectare), initial trinexapac acid residues on leaves were 0.29 and 0.44 mg kg - 1 , respectively. Residues were observed even after 15 days of spray. At harvest time, the residues of trinexapac acid in grains were below LOQ (limit of quantification) at 30 g a.i. ha - 1 treatment whereas, at 60 g a.i.ha - 1 , the residues were found to be 0.02 mg kg - 1 . In straw, trinexapac acid residues were detected to be 0.05 and 0.08 mg kg - 1 at 30 and 60 g a.i. ha - 1 treatments, respectively. The soil samples showed 0.04 and 0.08 mg kg - 1 residue at 30 and 60 g a.i. ha - 1 , respectively. The half life calculated for trinexapac acid came to be 10.10 and 9.09 days revealed the slow dissipation of trinexapac acid in paddy crop. The residue of trinexapac acid reached below LOQ at harvest time. Therefore the recommend dose of trinexapac ethyl is considered safe from consumption point of view., Competing Interests: Declarations. Conflict of 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., (© 2024. The Author(s), under exclusive licence to Springer Science+Business Media, LLC, part of Springer Nature.)

Resins have been used as remedies since ancient times and various embalming resins have been identified in recent years. In Europe, Mumia vera aegyptiaca, a resinous substance from ancient Egyptian mummies, was even sold in pharmacies as a tonic until the early 20th century. It is difficult to examine the composition of these archeological samples in detail as the well-established analytical techniques, that is, gas chromatography-mass spectrometry or liquid chromatography coupled with tandem mass spectrometry, are destructive and therefore do not allow the analysis of valuable archeological samples. Hence, there is an urgent need for alternative, nondestructive methods for the identification of resin residues. This study aims to explore and compare the use of five spectroscopic methods as an alternative to established analytical procedures. For that, 15 resin samples of known origin and three samples from an Egyptian market were studied. While laser induced-breakdown spectroscopy and terahertz time-domain spectroscopy provide only limited information for resin classification, nuclear magnetic resonance spectroscopy and Fourier-transform infrared spectroscopy can be used to classify the resin samples more accurately. Furthermore, photoluminescence/photoluminescence excitation spectroscopy shows a promising potential in combination with its general advantages, such as cost-efficiency, nondestructive nature, and fast data acquisition., (© 2024 The Author(s). Archiv der Pharmazie published by Wiley-VCH GmbH on behalf of Deutsche Pharmazeutische Gesellschaft.)