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JOURNAL OF FOOD PROTECTION · 2017 · IF 1.417

Simultaneous Determination of Isopyrazam and Azoxystrobin in Cucumbers by Liquid Chromatography–Tandem Mass Spectrometry

Dan Hu,Xu Xu,Tian Cai,Wei-Ying Wang,Chun-Jie Wu,Li-Ming Ye

ABSTRACT A rapid and sensitive analytical method based on high-performance liquid chromatography–tandem mass spectrometry was developed and validated for the determination of isopyrazam (IZM) and azoxystrobin (AZT) in cucumbers. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used as the pretreatment procedure. The samples were extracted with acetonitrile and cleaned up with octadecylsilyl silica (C18) and graphite carbon black. The proposed method resulted in satisfactory recovery of IZM and AZT (91.48 to 114.62%), and relative standard deviations were less than 13.1% at fortification concentrations of 1, 20, and 500 μg kg −1 ( n = 3). The limits of quantification for IZM and AZT were 0.498 and 0.499 μg kg −1 , respectively, which are far below the maximum residue level (0.5 mg kg −1 ) established for this type of sample. Matrix effects were also evaluated. This study established a sensitive and fast method for the detection of IZM and AZT in cucumber samples.

CAS / MDL: 30516-87-1
研究领域: 食品科学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD CHEMISTRY · 2020 · IF 6.306

Pesticide multi-residues in Dendrobium officinale Kimura et Migo: Method validation, residue levels and dietary exposure risk assessment

Zhenlan Xu,Lingxiangyu Li,Yi Xu,Shanshan Wang,Xiaoxia Zhang,Tao Tang,Jianzhong Yu,Huiyu Zhao,Shenggan Wu,Chunrong Zhang,Xueping Zhao

Dendrobium officinale Kimura et Migo ( D. officinale ) is a dual-use plant with both botanical medicine and food applications, drawing increasing attentions. Pesticides are inevitably applied on D. officinale in commercial artificial-sheltered cultivation, yet little is known about pesticide residue levels in D. officinale . A modified high through-put QuEChERS method coupled with HPLC-MS/MS was developed and validated to detect 76 pesticides in D. officinale . Graphitized multi-wall carbon nanotubes (g-MWCNTs) was selected as the clean-up sorbent, showing relative weak affinity to triazole fungicide having planar structure in their molecular and low matrix effects of pesticides in D. officinale samples compared to MWCNTs and pesticarb. The validated method was applied to analyze pesticide residues in 86 real D. officinale samples collected from three main producing provinces. 43 different pesticides were detected with highest residue of 6.11 mg/kg for dimethomorph. Given possible health risks related to pesticide residues, accordingly, risk assessment of human exposure to pesticides via intake of D. officinale was thus performed, indicating that the pesticide residue in fresh or dry D. officinale would not cause potential risk to human health either in the long-term or short-term. This work improved our understanding of potential exposure risk of pesticide multi-residues in D. officinale .

CAS / MDL: 1314-23-4
研究领域: 药用植物学 · 食品科学 · 分析化学 · 毒理学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2022 · IF 5.895

Establishment of a Method for the Detection of Indaziflam, Spirotetramat, Cyantraniliprole, and Their Metabolites and Application for Fruit and Vegetable Risk Assessment

Siwei Wang,Xiaonan Wang,Hong Chang,Haibin Sun,Yanping Liu

The presence of pesticides in foodstuffs has received increasing amount of attention worldwide. In this study, an efficient and sensitive QuEChERS/HPLC-MS/MS-based method was established for the simultaneous detection of indaziflam, cyantraniliprole, spirotetramat, and their metabolites on fruits and vegetables. The purification procedure and detection condition parameters were optimized. Good precision and reproducibility were found for the method, and the average recoveries of the target analytes ranged from 71 to 118%, with the relative standard deviation ranging from 2 to 12%. The limits of quantification and the limits of detection were 1–5 and 0.3–1.5 μg kg–1, respectively. The proposed method was used to detect three pesticides and their metabolites in fruit and vegetable samples collected from China’s major producing regions. Furthermore, the dietary risk posed by the pesticide residues on fruits and vegetables was evaluated by risk quotients (RQs) and risk probabilities (RPs). The RQ and RP values were less than 100% for Chinese consumers. This study not only provides a reliable analytical method for monitoring purposes but also serves as a significant guide for food safety and export.

CAS / MDL: 64-18-6 1314-23-4
研究领域: 食品安全 · 分析化学 · 毒理学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH · 2023 ·Vol. 30 ·期 35 ·84778-84790 · IF 5.8

Simultaneous determination of residues of multiple pesticides and their metabolites in citrus and orange juice from markets in China: residue levels and dietary risk assessment

Li Wei,Hou Huizhen,Hu Jiye

Consumers are becoming more concerned about pesticide residues in food. Since citrus represent a significant portion of the diet, it is appropriate to monitor the pesticide residues in citrus. In this paper, we modified a QuEChERS method combined with HPLC-MS/MS to investigate residue levels of 15 pesticides and 3 metabolites in citrus (whole fruit and pulp) and orange juice from the markets in China. And the dietary exposure risks were evaluated by using the hazard quotient (HQ) and hazard index (HI) methods based on deterministic and probabilistic models. The recoveries of the modified method ranged from 70 to 112% at three spike levels of 0.005–0.5 mg/kg with relative standard deviations of 1.0–18.1%. Pesticide residues were detected in 85.84% of the whole citrus and 40.00% of pulp, with concentrations ranging from 0.005 to 0.47 mg/kg, which did not exceed their maximum residue limits (MRLs) in China. The HQ (0.01–11.41%) and HI (0.07–16.2%) were both less than 100%, demonstrating that chronic, acute, and cumulative dietary risks were acceptable. Notably, the risk for children (1–6 years old, 1.96–16.2%) was higher than that for the general population (0.76–6.25%). The results of our study can provide a valuable reference for regular monitoring to protect public health and ensure pesticide management.

CAS / MDL: 7647-14-5
研究领域: 食品安全 · 分析化学 · 公共卫生
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Food Bioscience · 2024 · IF 4.8

Application of silanized melamine sponges in matrix purification for rapid analysis of multiple pesticides and veterinary drugs in honey by UPLC-MS/MS

Baocheng Ji,Lanrui Yang,Mengxian Zhang,Peiyu Li,Zhuchen Hou,Jia Lv,Xu Xu,Wenbao Bi,Gaigai Xu,Yanhong Bai

In this study, a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method based on two kinds of silanized melamine sponges coupled with ultra-high liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) were developed for the determination of multiple pesticides and veterinary drugs in honey. Quick and convenient matrix separation could be achieved with the developed silanized melamine sponges by simply soaking and squeezing. At three spiked levels, all recoveries of the monitored drugs ranged from 63.6% to 114.8%, with relative standard deviations less than 17.7%. No significant matrix influence was observed with matrix effects within −13.9%∼+15.1% for all monitored drugs. Good linearity with correlation coefficient (R 2 ) ≥0.991 was obtained in the range of 0.08–100 μg kg −1 for most drugs. The limits of detection and quantification ranged from 0.04 to 3.6 μg⋅kg −1 and from 0.08 to 9.8 μg⋅kg −1 , respectively. The results had shown the satisfactory matrix purification performance of silanized melamine sponges and indicated its good application prospect in the multiple determination of pesticides and veterinary drugs in various foods.

研究领域: 食品科学 · 分析化学
✓ 已验证 产品关联 DOI 高影响因子
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SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY · 2021 · IF 4.098

Rapid detection of sulfonamide antibiotics residues in swine urine by surface-enhanced Raman spectroscopy

Lulu Xu,Ruimei Wu,Xiang Geng,Xiaoyu Zhu,Yao Xiong,Tao Chen,Shirong Ai

Surface enhanced Raman spectroscopy (SERS) combined with rapid pretreatment technique was used to determine sulfonamide antibiotics (sulfadiazine and sulfathiazole) residue in swine urine. Au nanoparticles (AuNPs) were synthesized as Raman enhance substrate and the extraction of swine urine was purified with primary secondary amine (PSA), octadecyl silane (C 18 ) and graphitized carbon (GCB) to eliminate the interference of the matrix and different dosages of adsorbents (PSA, C 18 , GCB) were investigated. The results showed that the treatment with C 18 of 150 mg, GCB of 200 mg and PSA of 200 mg were an excellent approach for rapidly detecting sulfonamide antibiotics residue in swine urine. Combined with density functional theory calculation (DFT), Raman characteristic peaks of 819, 1102, 1173, 1588 cm −1 and 825, 1127 cm −1 were selected for qualitative and quantitative assessment of sulfadiazine and sulfathiazole in swine urine, respectively. Based on raman characteristic peak of 819 cm −1 , a good linear relationship between sulfadiazine concentration and Raman intensity was developed with R 2  = 0.9912, and based on raman characteristic peak of 825 cm −1 , a good linear relationship between sulfathiazole concentration and Raman intensity was developed with R 2  = 0.9941. And recoveries for five unknown concentration samples predicted were 98.47 ∼ 105.18% with relative standard deviation (RSD) of 1.53% ∼ 5.18%. This study demonstrated that SERS coupled with a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method could be employed to rapidly examine the sulfonamide antibiotics residue in swine urine towards its quality and safety monitoring.

研究领域: 食品安全 · 分析化学 · 兽医学
✓ 已验证 DOI 高影响因子
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JOURNAL OF CHROMATOGRAPHY A · 2015 · IF 4.169

Magnetic “one-step” quick, easy, cheap, effective, rugged and safe method for the fast determination of pesticide residues in freshly squeezed juice

Hao-Bo Zheng,Jun Ding,Shu-Jian Zheng,Qiong-Wei Yu,Bi-Feng Yuan,Yu-Qi Feng

A “one-step” quick, easy, cheap, effective, rugged and safe (QuEChERS) method was proposed for pesticide residue analysis in freshly squeezed juice of fruits and vegetables. In this method, a new magnetic adsorbent prepared by simple physical blending was adopt, which could endow the sample mixture with magnetic separability. To achieve the best performance of the modified QuEChERS towards target analytes, the amounts of adsorbents were investigated. Under the optimized conditions, a simple, rapid and sensitive method for the determination of 11 pesticide residues in freshly squeezed juice was established by coupling modified QuEChERS to gas chromatography/mass spectrometry analysis. The limits of quantification of the proposed method for 11 pesticides ranged from 2.0 to 49.6   ng/g. Good linearities ( R value ≥0.9993) were achieved at different concentration ranges, and acceptable method reproducibility was obtained by evaluating intra- and inter-day precisions with the relative standard deviations being less than 8.5% and 13.5%, respectively. The recoveries were in the range of 70.3–114.1% at different concentrations for real samples. Compared with the traditional QuEChERS methods, extraction/partitioning and purification were integrated into one step in the proposed method, which thus was time-saving (within 3.5   min) with keeping good clean-up performance.

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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FOOD CHEMISTRY · 2024 · IF 8.5

Eco-friendly chitosan microspheres as a novel one-step sorbent for the rapid purification and determination of pesticides and veterinary drug multi-residues in aquatic products with HPLC-MS/MS

Ruidong Zhou,Yupeng Wen,Wendi Huo,Cong Kong,Guangxin Yang,Huan Liu,Chaoying Zhang,Yingchun Mu,Dongmei Huang,Jincheng Li

A modified QuEChERS method was developed to determine multi-class pesticide and veterinary residues in aquatic products. Chitosan microspheres were conveniently synthesized and utilized as the cleanup adsorbent in the QuEChERS procedure, showcasing rapid filtration one-step pretreatment ability for the determination of drug multi-residues in aquatic products. Compared to conventional synthetic sorbents, chitosan microspheres not only have good purification performance, but also have renewable and degradable properties. This novel sorbent worked well in the simultaneous determination of 95 pesticides and veterinary drug residues in aquatic products after being combined with an improved one-step vortex oscillating cleanup method. We achieved recoveries ranging from 64.0% to 115.9% for target drugs in shrimp and fish matrix. The limits of detection and quantification were 0.5–1.0 and 1.0–2.0 μg kg −1 , respectively. Notably, hydrocortisone was detected with considerable frequency and concentration in the tested samples, underscoring the necessity for stringent monitoring of this compound in aquatic products.

CAS / MDL: 9012-76-4 64-18-6
研究领域: 分析化学 · 环境科学 · 食品安全
✓ 已验证 产品关联 DOI PubMed 高影响因子
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ENVIRONMENTAL RESEARCH · 2024 · IF 7.7

A study of the pesticide residues in rapeseeds in China: Levels, distribution and health risk assessment

Qi Guo,Xiaofeng Yue,Xin Qi,Xinyao Feng,Xuefang Wang,Xiaofeng Hu,Fei Ma,Liangxiao Zhang,Peiwu Li,Li Yu

The aim of this survey was to evaluate the residue levels, distribution and exposure risk of the 38 most commonly used pesticides in rapeseed samples collected from the main production areas in China over a two-year period. The sampling area covered 12 provinces, including Guizhou, Shaanxi, Yunnan, Hunan, Jiangxi, Sichuan, Chongqing, Anhui, Henan, Hubei, Zhejiang, and Jiangsu provinces. The pesticide residues were determined using a QuEChERS (Quick Easy Cheap Effective Rugged and Safe) method coupled with gas chromatography-tandem mass spectrometry and liquid chromatography-tandem mass spectrometry. 8.4% of the rapeseed samples contained pesticides with a residue level ranging from 0.001 to 0.634 mg/kg. The detected analytes were imidacloprid , quizalofop-P-ethyl, thiamethoxam , paclobutrazol , prochloraz, tebuconazole , difenoconazole, s-metolachlor, carbofuran , and carbendazim . The concentrations of four analytes, including thiamethoxam, difenoconazole, carbendazim and prochloraz, exceeded the maximum residue level set by the Chinese government for rapeseed, with exceedance rates of 0.1%, 0.1%, 0.1%, and 1.1%, respectively. Based on the index of quality for residues (IqR) values, 91.6% of the total rapeseed samples had an IqR category of Excellent (IqR = 0). Only 1.5% of the tested samples were of inadequate quality. Furthermore, the assessment of chronic and acute exposure, as well as health risks associated with pesticide residues in rapeseed, was conducted for different age groups within the Chinese population, including adults (6–14 years), children (15–49 years), and the elderly (50–74 years). The results of this assessment indicated that pesticide residues in rapeseed cultivated in China are not expected to be of short- or long-term risks to the Chinese customers.

CAS / MDL: 64-18-6
研究领域: 食品安全 · 环境科学 · 毒理学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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MOLECULES · 2024 ·Vol. 29 ·期 3 ·567 · IF 4.2

Profiling of Volatile Compounds in ‘Muscat Hamburg’ Contaminated with Aspergillus carbonarius before OTA Biosynthesis Based on HS-SPME-GC-MS and DLLME-GC-MS

Yayun Guo,Zhe Wang,Yi He,Huanhuan Gao,Hongmei Shi

Aspergillus carbonariusis known to produce the carcinogenic ochratoxin A (OTA) in grapes. The metabolism process before OTA biosynthesis influences the content and composition of the volatile compounds in grapes. In this study, a self-established method based on QuEChERS coupled with high-performance liquid chromatography–fluorescence detection (HPLC-FLD) was used to determine the OTA levels during a seven-day contamination period. The results showed that OTA was detected on the second day after contamination withA. carbonarius. Thus, the first day was considered as the critical sampling timepoint for analyzing the volatiles in grapes before OTA biosynthesis. Additionally, the volatile compounds in grapes were analyzed using headspace solid-phase microextraction gas chromatography–mass spectrometry (HS-SPME-GC-MS) and dispersive liquid–liquid microextraction gas chromatography–mass spectrometry (DLLME-GC-MS). The corresponding data were evaluated via multivariate data analysis using projection methods, including PCA and OPLS-DA. The results indicated significant differences in the nine volatile compounds in grapes contaminated withA. carbonariusbefore OTA biosynthesis. The results of the Pearson correlation analysis showed positive correlations between ethyl acetate, styrene, 1-hexanol and OTA; (E)-2-hexenal and nerolic acid were negatively correlated with OTA. Overall, these findings provide a theoretical basis for the early prediction of OTA formation in grape and grape products using GC-MS technology.Keywords:volatile compounds;Ochratoxin A;QuEChERS-HPLC-FLD;HS-SPME-GC-MS;DLLME-GC-MS;OPLS-DA

CAS / MDL: 7782-42-5
研究领域: 食品科学 · 真菌学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY A · 2013 · IF 4.612

Quick, easy, cheap, effective, rugged and safe method with magnetic graphitized carbon black and primary secondary amine as adsorbent and its application in pesticide residue analysis

Hao-Bo Zheng,Qin Zhao,Jie-Zhen Mo,Yun-Qing Huang,Yan-Bo Luo,Qiong-Wei Yu,Yu-Qi Feng

By using magnetic graphitized carbon black and primary secondary amine (GCB/PSA/MNPs) as adsorbent, a modified quick, easy, cheap, effective, rugged and safe (QuEChERS) method was proposed for pesticide residue analysis in vegetables. The magnetic adsorbent was fabricated via simple co-mixing method based on an “aggregate warp” mechanism. To achieve the optimum conditions of modified QuEChERS toward target analytes, several parameters, including the composition of analyte protectants and the amount of the adsorbents were investigated. Under the optimized conditions, a simple, rapid and effective method for the determination of 10 pesticide residues in vegetables was established by coupling modified QuEChERS to gas chromatography/mass spectrometry analysis. The detection limits of the proposed method for 10 pesticides ranged from 0.39 to 8.6   ng/g. Good linearity ( R value   ≥   0.990) was achieved at concentration levels of 10–200   ng/g, and acceptable method reproducibility was found as intra- and inter-day precisions, yielding the relative standard deviations less than 10.7% and 13.4%, respectively. The recoveries were in the range of 69.9–125.0% at different concentrations for real samples. Compared with the reported methods for the determination of a large number of samples, the proposed method has the advantage of less time-consuming in clean-up procedure.

CAS / MDL: 50-70-4
研究领域: 食品科学 · 环境科学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY A · 2017 · IF 3.981

Facile synthesis of amine-functional reduced graphene oxides as modified quick, easy, cheap, effective, rugged and safe adsorbent for multi-pesticide residues analysis of tea

Guicen Ma,Minglu Zhang,Li Zhu,Hongping Chen,Xin Liu,Chengyin Lu

Amine-functional reduced graphene oxide (amine-rGO) with different carbon chain length amino groups were successfully synthesized. The graphene oxides (GO) reduction as well as amino grafting were achieved simultaneously in one step via a facile solvothermal synthetic strategy. The obtained materials were characterized by X-ray diffraction, Raman spectroscopy, Fourier-transform infrared spectrometry and X-ray photoelectron spectroscopy to confirm the modification of GO with different amino groups. The adsorption performance of catechins and caffeine from tea acetonitrile extracts on different amine functional rGO samples were evaluated. It was found that tributylamine-functional rGO (tri-BuA-rGO) exhibited the highest adsorption ability for catechins and caffeine compared to GO and other amino group functional rGO samples. It was worth to note that the adsorption capacity of catechins on tri-BuA-rGO was 11 times higher than that of GO (203.7   mg   g −1 vs 18.7   mg   g −1 ). Electrostatic interaction, π-π interaction and surface hydrophilic-hydrophobic properties of tri-BuA-rGO played important roles in the adsorption of catechins as well as caffeine. The gravimetric analysis confirmed that the tri-BuA-rGO achieved the highest efficient cleanup preformance compared with traditional dispersive solid phase extraction (dSPE) adsorbents like primary-secondary amine (PSA), graphitized carbon black (GCB) or C18. A multi-pesticides analysis method based on tri-BuA-rGO is validated on 33 representative pesticides in tea using gas chromatography coupled to tandem mass spectrometry or high-performance liquid chromatography coupled with tandem mass spectrometry. The analysis method gave a high coefficient of determination (r 2   >   0.99) for each pesticide and satisfactory recoveries in a range of 72.1–120.5%. Our study demonstrated that amine functional rGO as a new type of QuEChERS adsorbent is expected to be widely applied for analysis of pesticides at trace levels.

研究领域: 分析化学 · 食品科学 · 环境科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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