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Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment · 2023 · IF 2.9

Residue levels and dietary risk evaluation of prothioconazole-desthio and kresoxim-methyl in cucumbers after field application in twelve regions in China

Chao Dong,Jiye Hu

A commercial formulation called prothioconazole·kresoxim-methyl 50% water dispersible granule (WG), used to control the powdery mildew, is under registration for use on cucumbers. Therefore it is urgent to validate the reliability of the recommended good agricultural practices (GAP) conditions (187.5 g a.i. ha−1, three sprays with a 7-d interval, and a pre-harvest interval of 3 d) by conducting field trials in 12 regions in China, as required by national regulations, with a subsequent risk assessment. The residues of prothioconazole-desthio and kresoxim-methyl in field samples were determined using QuEChERS coupled with high-performance liquid chromatography – tandem mass spectrometry (HPLC-MS/MS). On the suggested pre-harvest interval (PHI, 3 d), the residual concentrations of prothioconazole-desthio (no maximum residue limit set in China) and kresoxim-methyl (maximum residue limit = 0.5 mg/kg) in cucumbers were 0.01–0.020 and 0.01–0.050 mg/kg, respectively. The acute risk quotients of prothioconazole-desthio in cucumbers were no higher than 0.079% for Chinese consumers. The chronic dietary risk quotient of kresoxim-methyl and of prothioconazole-desthio for different groups of consumers in China ranged from 2.3% to 5.3% and from 1.6% to 4.6%, respectively. Thus, prothioconazole·kresoxim-methyl 50% WG sprayed on cucumbers under the recommended GAP information can pose a negligible risk for Chinese consumers.

CAS / MDL: 75-05-8 64-18-6
研究领域: 植物保护 · 食品安全
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment · 2024 · IF 2.3

Dissipation and residue of triadimefon in Rosa roxburghii

Lei Han,Zhaochun Jiang,Xuefei Zhang,Xiaomao Wu

Rosa roxburghii (R. roxburghii) is a unique, edible, medicinal fruit rich in vitamin C found in Southwest China. Triadimefon (TDF) is a triazole fungicide that is widely used to control powdery mildew in R. roxburghii. To assess the safety of TDF in R. roxburghii, an LC-MS/MS method was developed for the simultaneous quantification of TDF and its major metabolite, triadimenol (TDN) in R. roxburghii. Both TDF and TDN showed high correlation coefficients (>0.999) for the solvent- and matrix-matched calibrations. The recovery rates of TDF and TDN in R. roxburghii ranged from 90.18% to 100.42%, with a relative standard deviation (RSD) of 1.25%–9.22%. The limit of quantification (LOQ) was 0.01 mg·kg−1. The half-life of TDF in R. roxburghii was between 2.74 and 3.07 days, with terminal residues ranging from < LOQ to 1.84 mg·kg−1. Recommended maximum residue limits (MRLs) and safe pre-harvest intervals (PHIs) for TDF in R. roxburghii were 0.5 mg·kg−1 and 21 days, respectively. This study provides essential data for TDF’s safe and judicious use in R. roxburghii production.

研究领域: 植物保护 · 分析化学 · 食品安全
✓ 已验证 DOI PubMed 高影响因子
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INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY · 2020 · IF 1.431

Residues, fate and risk assessment of spirotetramat and its four metabolites in pineapple under field conditions

Yiran Liang,Wenxia Wu,Xiaojun Cheng,Jiye Hu

The aim of this study was to investigate the fate, terminal residues and risk assessment of spirotetramat and its four metabolites in pineapple and pineapple pulp samples. To achieve this goal, a simple, efficient and sensitive method based on QuEChERS technique was developed using LC-MS/MS. The limit of quantification was 0.01 mg/kg for all the target analytes with the average recoveries ranging from 77% to 109%. The validated method was successfully applied to investigate the fate and terminal residue of spirotetramat and its four metabolites in pineapple and pineapple pulp samples in China. The dissipation dynamics of spirotetramat in pineapple were investigated according to first-order kinetics and the calculated half-lives were 4.6 and 2.3 days in the two sampling locations. After two or three applications at the doses of 80 to120 mg a.i./kg, the highest spirotetramat residue (sum of spirotetramat and its four metabolites) that detected in pineapple and pineapple pulp samples were 0.203 and 0.064 mg/kg. The dietary risk assessment of spirotetramat in pineapple was assessed by risk quotients and the calculated risk quotient value was found to be far below 100%, indicating a low health risk to the consumers. As there was no recommended MRL value in pineapple in China, these results should be useful for safe and reasonable usage of spirotetramat in pineapple in China.

CAS / MDL: 203313-25-1
研究领域: 食品科学 · 环境科学 · 毒理学
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BULLETIN OF ENVIRONMENTAL CONTAMINATION AND TOXICOLOGY · 2023 ·Vol. 111 ·期 4 ·1-9 · IF 2.7

The Dissipation Kinetics, Residue Level and Dietary Risk of Kresoxim-Methyl in Rosa roxburghii and Soil Based on the QuEChERS Method Coupled with LC–MS/MS

Zheng Handinghong,Wu Qiong,Wu Xiaomao

This study aimed to investigate the dissipation, residues and dietary assessment of kresoxim-methyl in the application of Rosa Roxburghii and soil field using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The results show that kresoxim-methyl in R. roxburghii samples was extracted by acetonitrile and purified by ethyl enediamine-N-propylsilane (PSA), while kresoxim-methyl in soil samples was extracted by acetonitrile and purified by octadecylsilyl solid phase dispersant (C 18 ). 0.1% formic acid (v/v)-water–methanol solution was used as the mobile phase, LC–MS/MS exhibited a good linearity in the range of 0.001–10 mg L −1 . The recoveries of R. roxburghii and soil matrix were 82.48%–102.55%, and the relative standard deviation ( RSD) were 1.13%–4.21%. The limit of detection ( LOD ) and quantification ( LOQ ) of kresoxim-methyl in R. roxburghii and soil samples was 0.50 and 0.60 µg kg −1 , respectively. The dissipation dynamics of kresoxim-methyl in R. roxburghii and soil followed the first-order kinetics, with the half-life of 4.28 and 4.41 days, respectively. The terminal residual amount of kresoxim-methyl in R. roxburghii and soil samples was 0.003–1.764 and 0.007–2.091 mg kg −1 , respectively. The dietary intake risk assessment indicates that a risk quotient ( RQ ) for kresoxim-methyl based on the national estimated daily intake ( NEDI ) of 0.1995 mg was 0.79%, suggesting that the use of kresoxim-methyl on R. roxburghii at recommended dosage was safe to consumers. This study provides the theoretical basis for guiding the rational use of kresoxim-methyl in the production of R. roxburghii .

CAS / MDL: 64-18-6 143390-89-0
研究领域: 植物学 · 农业科学 · 食品科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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ACS Omega · 2023 · IF 4.1

Determination of the Dissipation Dynamics and Terminal Residue of Bupirimate and Its Metabolites in Cucumber by QuEChERS-Based UPLC-MS/MS

Yue Chen,Deliang Gao,Yueming Wu,Ling Wang,Weidi Fan,Yun Gao,Wenli Wang,Li Su,Beixing Li,Wei Mu,Weili Yu

Bupirimate is widely used as a highly active systemic fungicide. However, the frequent and heavy use of bupirimate has led to pesticide residues in crops that threaten human health and food safety. At present, there is limited research on the detection of ethirimol, which is the metabolite of bupirimate. This study established an ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method to simultaneously detect bupirimate and ethirimol residues based on QuEChERS pretreatment. The average recoveries of bupirimate and ethirimol in cucumber were between 95.2 and 98.7%, respectively, with relative standard deviations (RSDs) of 0.92–5.54% at fortified levels of 0.01, 0.1, and 5 mg L–1. The established method was used to determine the residues in field trials in 12 regions of China, and the final residues of bupirimate were all less than the maximum residue limit (MRL). Since the risk quotient (RQ) of bupirimate and ethirimol in cucumber was less than 1.3%, the dietary risk assessment indicated that bupirimate and ethirimol had a low long-term dietary risk to the general population in China. This study provides effective guidance on the proper use of bupirimate in cucumber fields and a reference for establishing the MRL of bupirimate in China.

CAS / MDL: 64-18-6
研究领域: 植物保护 · 食品安全 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD CHEMISTRY · 2024 · IF 8.5

Underestimation of tetracycline antibiotic residues in chicken meat: The role of protein binding

Aying Wen,Huihui Wang,Shaofeng Yuan,Hang Yu,Yahui Guo,Weirong Yao

Interesting variations in the analyte content were observed in chicken samples contaminated with tetracycline antibiotics (TCs) following pretreatment with various enzymatic hydrolysis before quantification by conventional analytical methods. Compared with untreated samples, the detectable contents of three TCs in protease-treated samples were 1.51 to 2.05 times higher, whereas lipase treatment did not significantly influence the contents. The marked changes following protease treatment confirmed the presence of protein-associated antibiotics. Infrared spectroscopy analysis indicated that the formation of protein-bound antibiotics resulted from non-covalent interactions between TCs and proteins. Further dissociation experiments determined that the intermolecular forces involved hydrogen bonding, hydrophobic interactions, and electrostatic attraction. Molecular docking substantiated these forces and detailed the binding mechanism at the molecular level. Moreover, the masking effect of protein binding on the determination of TCs was also evidenced in an additional 30 positive chicken samples, suggesting that the actual residue levels of TCs in protein-rich foodstuffs are underestimated.

研究领域: 食品安全 · 分析化学 · 药理学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY · 2022 · IF 2.731

Residue dissipation and dietary risk assessment of fluopyram and its metabolite (M25) in melon

Feng Yizhi,Zhang Aijuan,Pan Jinju,Zuo Bojun,Liang Lin

The aim of this study was to investigate the dissipation and residues of fluopyram in melon under field conditions and to assess its safe use. A liquid chromatography tandem mass spectrometry (LC-MS/MS) with QuEChERS for analysis of fluopyram and its metabolite M25 was established. Under the experimental condition of adding different levels of analytes (0.02 ~ 2 mg kg−1), the average residue recovery of fluopyram and M25 in melon was 96%~105% with a relative standard deviation of 2%~8%. The limit of quantitation of fluopyram and M25 in melon was 0.02 mg kg−1. Field trial results showed that the half-life of fluopyram in melon was 4.5–6.2 days, and the degradation was relatively fast. The residual of M25 in melon was lower than the LOQ. The terminal residues of fluopyram in melon sample were in the range of <0.02 ~ 0.095 mg kg−1, which was lower than the maximum residue limit for melon in EU (0.4 mg kg−1) and South Korea (0.6 mg kg−1). Dietary risk assessment indicated that the long-term intake risk quotient (rqchronic) and short-term intake risk quotient (rqacute) of fluopyram in people from different age groups were 0.000079 ~ 0.000671 and 0.002978 ~ 0.025268, respectively, which were significantly lower than 1. Therefore, the residues of fluopyram in melons would not affect the health of the general population in China.

CAS / MDL: 360-64-5
研究领域: 植物保护学 · 食品安全 · 分析化学
✓ 已验证 产品关联 DOI 高影响因子
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ANALYTICAL LETTERS · 2024 · IF 1.6

Sensitive Determination of Carbendazim in Tobacco Leaves by Surface Enhanced Raman Spectroscopy (SERS) Using a Silica – Silver Nanoparticle Substrate and QuEChERs Pretreatment

Zheng Feng,Xue Yang,Xiaowei Guo,Jiamin Yu,Fan Li,Jimin Shao,Hui Liang,Hong Jiang

A sensitive surface enhanced Raman spectroscopy (SERS) substrate based on SiO2@Ag core-shell with a QuEChERs pretreatment method were constructed for the determination of carbendazim residue in tobacco leaves. The SERS substrate was formed by self-assembly of monolayer homogeneous SiO2 nanospheres onto silicon wafer following by vacuum thermal evaporation of silver film. The QuEChERs pretreatment method was used to eliminate the interfering effects of pigments and organic acids in tobacco leaves. The results for carbendazim in tobacco leaves show the limit of detection (LOD) of the SERS substrate was 0.1 mg/kg and the recovery rate was from 82.56% to 95.93%. The proposed low-cost sensitive SERS substrates provide potential application for tobacco safety monitoring.

CAS / MDL: 10605-21-7 78-10-4
研究领域: 分析化学 · 食品安全
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INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY · 2021 · IF 2.826

Residue determination and risk assessment of benziothiazolinone in citrus by LC-MS/MS

Xiangwu Liu,Bangyan Song,Xiaoxia Jiang,Ya Yang,Ping Lu,Deyu Hu

A quick, easy, cheap, effective, rugged and safe liquid chromatography-tandem mass spectrometry technology was used to determine benziothiazolinone in citrus. Orthogonal test and single-factor analysis were conducted to identify the optimal extraction method of benziothiazolinone. The good linearity (R2 > 0.9949), high accuracy and precision, matrix effect and satisfactory recoveries (79.31%–98.68%) at three spiked levels (0.02, 0.2 and 2 mg/kg) with low relative standard deviation values (0.63%–8.68%) were validated. The limits of detection and quantification were within 0.2–0.8 and 20 μg/kg, respectively. This study could provide guidance for the reasonable use of this fungicide and for the establishment of maximum residue level.

研究领域: 食品科学 · 分析化学
✓ 已验证 DOI 高影响因子
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS · 2023 · IF 4.3

Residue and dietary risk assessment of glyphosate, glufosinate-ammonium, and their metabolites in maize and soybean

Kuan Wang,Bin Jiao,Haixiang Gao,Xinglu Pan,Xiaohu Wu,Jun Xu,Fengshou Dong,Yongquan Zheng

Persistent weed growing in herbicide-resistant maize and soybean fields is controlled increasingly by glyphosate (GLY) and glufosinate-ammonium (GLU). There is increasing concern that consumers may be exposed to herbicide residues . A Total of 224 samples involved supervised trials and market sampling were carried out. And the levels of GLY and GLU were determined in maize and soybean samples by UPLC−MS/MS method. The residues of GLY and GLU were at a low level in all samples and ranged from <0.04 to 0.29 mg/kg and <0.04 to 0.91 mg/kg, respectively. Deterministic and probabilistic models were used to assess the dietary risk, and the highest risk quotient (RQ) values of GLY and GLU were 2.24 × 10 −4 and 3.27 × 10 −2 , respectively. The RQs of GLU are significantly higher than that of GLY. Risk assessment results showed that GLY and GLU residues should not pose serious health risks to Chinese consumers.

CAS / MDL: 1066-33-7
研究领域: 农业科学 · 食品安全 · 毒理学
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Journal of Orthopaedic Translation · 2017 · IF 0

Quantitative determination of residual 1,4-dioxane in three-dimensional printed bone scaffold

Ling Li,Jing Long,Long Li,Huijuan Cao,Tingting Tang,Xinghua Xi,Ling Qin,Yuxiao Lai,Xinluan Wang

Summary Background/Objective A novel porous scaffold poly (lactide- co -glycolide) and tricalcium phosphate (PLGA/TCP) was developed by three-dimensional printing technology for bone defect repair. As a Class 2 solvent with less severe toxicity, content of residual 1,4-dioxane in this newly developed scaffold should be rigorously controlled when it is translated to clinical use. In this study, a headspace gas chromatography-mass spectrometric (HS-GC-MS) method and related testing protocol were developed for quantitative determination of 1,4-dioxane in the PLGA/TCP composite scaffolds. Methods Matrix effect analysis was used to optimise the pretreatment method of the scaffolds. Then, the procedure for testing 1,4-dioxane using HS-GC-MS was set up. The accuracy, precision, and robustness of this newly developed quantitative method were also validated before quantification of 1,4-dioxane in the scaffolds with different drying procedures. Results Dimethyl formamide (DMF) was the optimal solvent for dissolving scaffolds for GC-MS with proper sensitivity and without matrix effect. Then, the optimised procedure was determined as: the scaffolds were dissolved in DMF and kept at 90°C for 40 minutes, separated on a HP-5MS column, and detected by mass spectroscopy. Recovery experiments gave 97.9–100.7% recovery for 1,4-dioxane. The linear range for 1,4-dioxane was determined as 1–40 ppm with linear correlation coefficient ≥ 0.9999. Intraday and interday precision was determined as being within relative standard deviation of below 0.68%. The passable drying procedure was related to lyophilising (−50°C, 50 Pa) the scaffolds for 2 days and drying in vacuum (50 Pa) for 7 days. Conclusion This is the first quantitative method established to test 1,4-dixoane in a novel scaffold. This method was validated with good accuracy and reproducibility, and met the methodological requirements of the Guideline 9101 documented in the Chinese Pharmacopoeia 2015 Edition. The translational potential of this article This quantitative method for determination of residual 1,4-dioxane in the novel scaffolds is a key technical method during its translation into clinical use because this method is an important and indispensable file in the enterprise standard when the porous scaffold is registered as a Class III implanted medical device for bone defect repair, which is used to guarantee the safety of the scaffolds. It is also applied to optimise the drying process of scaffolds and to monitor the quality of scaffolds in the industrialisation process. Further, this method provides references for other solvents quantitative determination in porous scaffolds or materials.

研究领域: 生物材料学 · 分析化学 · 医学工程
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WATER AIR AND SOIL POLLUTION · 2023 ·Vol. 234 ·期 2 ·1-16 · IF 2.9

Residues and Bioavailability of Neonicotinoid Pesticide in Shaanxi Agricultural Soil

Hua Li,Zhao Danyang,Wang Huining,Wei Ting

Shaanxi is an important agricultural province in China. The rapid development of agriculture has led to an increase in the use of pesticides, which has resulted in a serious pesticide pollution problem. In addition, assessing the total residue concentrations would overestimate the actual hazard of neonicotinoid pesticides, so it is essential to study the bioavailability of neonicotinoid pesticides. In the study, 115 soil samples collected from different areas from northern, central, and southern Shaanxi were used to determine the residues of four neonicotinoid pesticides: imidacloprid, acetamiprid, clothianidin, and thiamethoxam. An analytical method applied to assess the bioavailability of neonicotinoid pesticides was established, the bioavailability of different types of neonicotinoid pesticides and related factors affecting their bioavailability were determined, and the changes in the bioavailability of neonicotinoid pesticides in actual and simulated soils were explored. The results showed that the detection rates and residue levels of neonicotinoid pesticides varied in different regions of Shaanxi. By studying the bioavailability of neonicotinoid pesticides, it was found that the bioavailability of the four neonicotinoid pesticides was always: thiamethoxam > acetamiprid > imidacloprid > clothianidin, which may be related to their structural properties. Soil pH is positively related to the size of the bioavailability of neonicotinoid pesticides, while soil organic matter content and soil aging time are negatively related to the size of the bioavailability of neonicotinoid pesticides.

研究领域: 环境科学 · 农业科学 · 毒理学
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