FOOD CHEMISTRY
·
2021
·
IF 7.514
Yan Yang,Guobing Lin,Lijing Liu,Tainan Lin
Antibiotic residues in honey cause public health problems. To analyze multi-antibiotic residues in honey, a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction method coupled with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed for simultaneous quantification of 70 antibiotic residues in honey. Matrix-matched calibrations indicated the correlation coefficients were higher than 0.998. The recovery was in a range of 70.5%-119.8% with intra-day relative standard deviation (RSD) of ≤ 10.0% and inter-day RSD of ≤ 13.9%. The limits of detection ranged between 0.050 μg/kg and 1.02 μg/kg. Limits of quantification was 0.17 μg/kg to 3.40 μg/kg. The matrix effects were negligible in 71.4% of compounds and moderately in 24.3% of compounds. Methacycline, oxytetracycline, tetracycline and its metabolite 4-tetracycline residues were detected in the tested samples. Validation parameters were acceptable and were in line with the Codex guidelines. This method was effective for detecting multi-antibiotic residues in honey.
研究领域:
食品科学
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分析化学
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公共卫生
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2023
·
IF 8.8
Youzhi Su,Jianjiang Lu,Jun Liu,Fang Li,Ning Wang,Hongqin Lei,Xiaofang Shen
A modified QuEChERS purification–liquid chromatography-tandem mass spectrometry method has been developed to determine 51 pesticide residues with newly established maximum residue limits (MRLs) in foodstuffs. Samples were extracted with acetonitrile under citrate-buffered conditions and purified using a modified QuEChERS method employing hydroxylated MWCNTs , SAX, and C 18 . The limits of quantification ranged from 0.2 to 9.8 µg/kg. Recoveries in ten different foodstuffs ranged from 70.2% to 117.9%, with relative standard deviations between 2.3% and 19.9% at three spiking levels. This method was applied to analyze 352 market samples, detecting 14 pesticides in 97 samples. Notably, Afidopyropen, cyantraniliprole, and fluxapyroxad residues in vegetables exhibited a consistent pattern of higher levels in the spring and winter and lower levels in the summer and autumn. Moreover, the risk assessments for acute and chronic dietary exposure to the 14 detected pesticides indicated that the %ADI and %ARfD were well below 100%.
研究领域:
分析化学
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食品安全
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环境科学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2022
·
IF 9.231
Meng Wang,Jingjing Wang,Kangkang Wang,Liugen Zhang,Xianglei Cao,Cheng Guo,Jide Wang,Bin Wu
More and more attention has been paid to the improved QuEChERS (quick, easy, cheap, effective, rugged and safe) method in dealing complex sample matrices, especially for the study of QuEChERS adsorbents. In this study, a magnetic mesoporous material, which was derived from MIL-88B modified by l -alanine, was synthesized as modified QuEChERS adsorbents for the simultaneous determination of multiple pesticides (Methomyl, Isoprocarb, Carbofuran, 3-Hydroxycarbofuran, Acetamiprid, Imidacloprid) in Chinese cabbage, celery, long bean and leek. The prepared magnetic adsorbents can effectively remove interfering substances from the sample, and the proposed modified QuEChERS method can reduce sample pretreatment time via an external magnetic field. To achieve the best performance of QuEChERS method, the clean-up time and amount of QuEChERS adsorbents were investigated. Under the optimized conditions, a simple, rapid and sensitive method for the determination of 6 pesticide residues in vegetables was established by coupling the modified QuEChERS to ultrahigh-performance liquid chromatography-tandem mass spectrometry. Excellent sensitivity (The limit of detection for the 6 pesticides ranged from 0.001 to 0.020 µg kg −1 ), satisfactory linearity (r 2 ≥ 0.9952), good recovery (73.9–107.7%) and good precision (3.6–16.9% for intraday relative standard deviation, 0.5–15.0% for interday relative standard deviation) were obtained. Compared with traditional QuEChERS method, the proposed method is simple, cost-effective, and efficient, which indicates that the method can be used to detect carbamate and neonicotinoid pesticides in real samples and provide an excellent pretreatment technique for the detection of trace multi-analytes from complex substrates.
研究领域:
分析化学
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食品安全
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2025
·
IF 9.8
Zi-Ling Li,Xiao-Run Qi,Yi-Heng Xu,Jia-Qi Zhao,Gui-Fu Zuo,Man-Man Wang
Effective and convenient QuEChERS of lipophilic pesticides with wide p K a range from strongly pigment-rich food samples remains a great challenge. Here, ZIF-67 derived magnetic nanoporous carbon (Co@MPC) was firstly proposed for modified QuEChERS of carbamate pesticides ( pK a 4.3–12.3) in various vegetable and fruit samples prior to LC-MS/MS. This sorbent offered superior adsorption capacities of 29.89 mg/g and 22.28 mg/g towards chlorophyll and lutein via π-π and hydrophobic interactions. The present method exhibited acceptable matrix effect of −4.8 %-14.4 %, low detection limits of 0.003–0.02 μg/kg and satisfactory recoveries of 80.2 %–108 % in celery, cabbage, Chinese cabbage, apple, banana and orange samples. 10 mg of Co@MPC enabled highly efficient matrix purification and isolation in 20 s, offering low-cost and facile clean-up process. The study highlighted great potential of Co@MPC as QuEChERS sorbent, and demonstrated its wide applicability and broad application prospects to monitor the contaminants in food items.
研究领域:
分析化学
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食品安全
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环境科学
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产品关联
DOI
PubMed
高影响因子
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2022
·Vol. 36
·期 12
·e9284
·
IF 2.586
Xi Lv,Fengzhong Wang,Ying Cui,Bei Fan,Zhiqiang Kong,Tingcai Yan,Minmin Li
Rationale Oil crops and products are important food materials in daily life. Pesticide residues in food could directly and indirectly endanger human health. However, the method for detecting multiple pesticides simultaneously is limited. In this study, an easy and efficient method for the simultaneous determination of 38 pesticides in oil crops and products was established and validated. Methods All samples were treated with a modified QuEChERS procedure followed by ultra-high-performance liquid chromatography/tandem mass spectrometry (UHPLC/MS/MS) analysis. Mass spectrometry was performed in positive and negative ion electrospray ionization mode. The mobile phase consisted of 0.1% formic acid in water and 0.1% formic acid in acetonitrile. The column used was a Poroshell 120 EC-C18 and the flow rate was 0.3 mL/min. Results The method was validated so that the calibration curves for all pesticides had good linearity in the concentration range of 10–1000 μg/L with correlation coefficients (R 2 ) above 0.9945. The recovery rates were between 70.1 and 120.0%, with relative standard deviations (RSDs) (n = 6) ≤20.0%. The limits of quantification (LOQs) ranged from 0.5 to 10 μg/kg, limits of detection (LODs) ranged from 2.0 to 30 μg/kg, and the matrix effect (ME) ranged from −18.77 to 19.33%, respectively. Conclusions The method proved to be accurate, sensitive, and stable. It can be used for rapid screening and confirmation of 38 pesticide residues in oil crops and products which takes 10 min for sample extraction and clean-up with less requirement of solvents. This study provides a technical basis for regulatory analysis and quality supervision of foods.
研究领域:
食品安全
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分析化学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2021
·Vol. 35
·期 12
·e5209
·
IF 1.902
Yunheng Yao,Longlv Bai,Haifeng Tian,Xinzi Wu,Nianjie Zhang,Lunpeng Wu,Yifan Jia,Xiuli Ren
In this study, a new fluorinated methacrylamide (MACF) was synthesized and evaluated as an adsorbent in the dispersive solid-phase extraction for the effective determination and extraction of 20 organophosphorus pesticides (OPPs) from ginseng samples using the QuEChERS (quick, easy, cheap, effective, rugged, safe) method coupled with GC–MS/MS. The properties of MACF were characterized using Fourier-transform infrared spectroscopy, elemental analysis, and high-resolution 19 F NMR. MACF, chitosan, primary and secondary amine, octadecylsilane, graphitized carbon black, Z-Sep, Z-Sep + , and EMR-Lipid were compared in terms of extraction efficiency. The best results were obtained when MACF was used. Matrix-matched calibration was employed for quantification. All the OPPs exhibited good linearity ( r 2 > 0.9969) with the concentration at their respective concentration ranges. The limits of detection were 1.5–3.0 μg/kg, and the limits of quantification were 5.0–10.0 μg/kg. The trueness of the 20 pesticides at four spiked levels ranged from 86.1 to 111.1%, and the relative standard deviation was less than 11.3%. The modified QuEChERS method using MACF as the adsorbent was sensitive, reliable, and cost-effective and could be used for the determination of 20 OPP residues in ginseng.
研究领域:
分析化学
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环境科学
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药学
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食品科学
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DOI
PubMed
高影响因子
Analytical Methods
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2025
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IF 2.6
Wei Chen,Xuanyu Hong,Huachun Liu,Ruifang Fan
Liquid crystal monomers (LCMs) are emerging organic pollutants to which humans are chronically exposed at low doses. Accurate quantification of LCMs in biological matrices remains challenging due to their low environmental concentrations and significant matrix effects. This study developed a novel approach for robust determination of three LCMs including 2,3-difluoro-4-(trans-4-propylcyclohexyl) butoxybenzene (3cH4OdFP), 4-propoxy-4′-cyanobiphenyl (3OCB), and 4-ethyl-4′-(4-propylcyclohexyl)-1,1′-biphenyl (3cH2B) in mouse serum, brain, heart, liver, spleen, lung, and kidney tissues. Serum samples were extracted with n-hexane, while tissues were extracted using acidified acetonitrile followed by QuEChERS cleanup.Separation was achieved on a DB-17HT column, and detection was performed in selected ion monitoring (SIM) mode of GC-MS. The method demonstrated good linearity (r² > 0.995) from 0.5 to 200 ng/mL. Limits of detection were 0.2 ng/g for tissues and 1.0 ng/mL for serum. Average recoveries ranged from 74.32% to 126.0%, with intra-day and inter-day precision between 2.165%-18.53% and 3.749%-19.13%, respectively. The validated method was successfully applied to exposed mice, revealing widespread tissue distribution of three LCMs, with the spleen showing a higher accumulation potential. This sensitive and reliable approach provides robust technical support for internal exposure assessment and toxicological studies of LCMs.
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PubMed
高影响因子
ANALYTICAL LETTERS
·
2025
·
IF 1.8
Yating Liu,Li Tian,Yuan Gao,Zhonghai Tang,Yuzhu Xiong
An attapulgite-multi-walled carbon nanotube (ATP-CNTs) composite material was synthesized to enhance the QuEChERS method. When coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), an accurate, rapid, and reliable analytical method was established for the determination of multiple pesticide residues in tea. The ATP-CNTs purification agent was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). Pesticides in tea were extracted under ultrasonication using water and acetonitrile, followed by purification with ATP-CNTs. Key experimental parameters—including extraction solvent, extraction time, soaking time, soaking water temperature, adsorbent combination ratio, and adsorbent amount—were systematically optimized. Under optimal conditions, the method’s limits of detection (LOD) and quantification (LOQ) were 1.05–4.11 μg/kg and 3.49–13.69 μg/kg, respectively. Recovery experiments at three spiked concentration levels yielded average recoveries ranging from 75.2% to 114.3%, with relative standard deviations (RSDs) between 2.3% and 13.8%. The results demonstrate that this method is simple, accurate, rapid, and suitable for the detection of relevant pesticide residues in tea.
研究领域:
分析化学
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环境科学
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食品科学
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纳米技术
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产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Liang Qi,Xinting Zhang,Longjiang Li,Xilan Li,Xiangna Chang
Prolonged use of cosmetics containing banned fluoroquinolones can cause skin disorders and increase drug resistance. The QuEChERS method holds considerable application prospect in the pretreatment of cosmetic samples. Although octadecyl (C 18 )-bonded silica sorbent is commonly used as a QuEChERS clean-up material, the conventionally commercially available bulk C 18 sorbent is relatively costly and has a limited purification mechanism. In this study, using dendritic silica sphere (dSiO 2 ) as the substrate, and through the condensation reaction between cyanuric chloride (CNCl) and the amino group, a dNSiO 2 -CNCl-C 18 sorbent was synthesized. The sorbent was characterized using infrared spectroscopy, transmission electron microscopy, surface area and pore size analysis, and water contact angle measurements. The experimental results regarding the matrix removal from the model cosmetic lotion showed that dNSiO 2 -CNCl-C 18 exhibited a higher matrix removal efficiency compared to a commercial C 18 sorbent. Furthermore, a QuEChERS-HPLC-FLD method was developed using dNSiO 2 -CNCl-C 18 for the simultaneous detection of four fluoroquinolones, norfloxacin (NOR), pefloxacin (PEF), enrofloxacin (ENR), and difloxacin (DIF). The linear ranges were 0.10 to 100.0 μg L −1 for NOR and PEF, and 0.05 to 100.0 μg L −1 for ENR and DIF, with coefficient of determination exceeding 0.999. Satisfactory spiked recoveries for the lotion sample ranged from 91.5% to 107.0%, with intra-day and inter-day precision values not exceeding 7.6%. The established method was subsequently validated through its successful application in additional cream and emulsion samples. dNSiO 2 -CNCl-C 18 exhibits low synthesis costs and demonstrates promising potential for matrix purification in various complex samples, facilitating the rapid determination of target compounds.
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PubMed
高影响因子
Journal of Analytical Methods in Chemistry
·
2025
·Vol. 2025
·期 1
·8995925
·
IF 2.2
Zejun Wang,Qingcheng Wang,Fei Xu,Linhua Wang,Jingjing Liang,Qing Shen,Shunyuan Guo
This study developed a method for simultaneously detecting 10 mycotoxins in Dendrobium officinale using the QuEChERS technique combined with ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS). The method was optimized for sample purification, pretreatment, chromatographic conditions, and mass spectrometric settings. It effectively addressed the matrix effects from impurities like pigments and cellulose. The validation of the method showed good linearity ( R 2 > 0.990), with limits of detection (LODs) ranging from 0.23 to 8.61 μg kg −1 and limits of quantification (LOQs) from 0.77 to 28.7 μg kg −1 . Average recoveries for the 10 mycotoxins ranged from 77.9% to 98.5%, with relative standard deviations (RSD) between 2.26% and 8.28%. The method demonstrated high accuracy, precision, and suitability for large-scale screening of mycotoxins in Dendrobium officinale. When applied to 84 samples, the contamination rate was 2.38%, with the main contaminants being AFB1, ZEN, and AFG1. This method provides a reliable, cost-effective approach for detecting mycotoxin contamination in traditional Chinese medicine.
研究领域:
分析化学
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中药学
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食品安全
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药物质量控制
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代谢组学
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毒理学
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产品关联
DOI
PubMed
高影响因子
Journal of Analytical Methods in Chemistry
·
2021
·
IF 2.193
Ling Yu,Guiquan Guo,Jun Zhao,Linnan Zhao,Aiqing Xia,Xu He,Cuijuan Xing,Lili Dong,Fang Wang
A fast method based on Fe3O4 magnetic nanoparticles (Fe3O4 MNPs) modified QuEChERS integrated to dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry was established for the determination of 8 organochlorine pesticides (OCPs) in green leafy vegetables. The factors involved in the purification by QuEChERS and concentration by DLLME were optimized. In the QuEChERS process, Fe3O4 MNPs were used as a new impurity adsorbent after the sample extraction procedure by acetonitrile, which achieved phase separation rapidly. Carbon black was used as an alternative to costly graphitized carbon black without affecting the recovery. In the process of DLLME, 1 mL of the extract obtained by QuEChERS was used as the dispersive solvent, 40 μL of chloroform was used as the extractive solvent, and 4 mL of water was added. Making them mix well, then the dispersed liquid-liquid microextraction concentration was subsequently carried out. The enrichment factors of 8 OCPs ranged from 22.8 to 36.6. The recoveries of the proposed method ranged from 78.6% to 107.7%, and the relative standard deviations were not more than 7.5%. The limits of detection and limits of quantification were 0.15–0.32 μg/kg and 0.45–0.96 μg/kg, respectively. The method has been successfully applied to the determination of OCPs in green leafy vegetable samples.
研究领域:
分析化学
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食品安全
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环境科学
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产品关联
DOI
PubMed
高影响因子
Separations
·
2023
·Vol. 10
·期 8
·459
·
IF 2.6
Xiaoqiong Wu,Yun Lin,Xiang Zhang,Nan Ouyang,Ying Zhou
The present study employed a modified QuEChERS method to systematically analyze the presence of fifteen quinolone and seven tetracycline antibiotic residues in local animal food. Additionally, a multi-level four-factor Box–Behnken design (BBD) within the framework of response surface methodology (RSM) was utilized to evaluate the factors impacting the detection efficiency of the sample pretreatment procedure. Optimization was performed via Design Expert®10.0.3, and the factors, including the volume of the acetonitrile, the addition of formic acid, the duration of the extraction, and the addition of EDTA, were combined with experimental design until an optimal solution was reached. Finally, the sample was tested via ultra-high performance liquid chromatography-quadrupole-linear ion trap mass spectrometry (UPLC/MS/MS) in both multiple reaction monitoring (MRM) and enhanced product ion (EPI) scan modes on a QTRAP®5500 instrument (AB SCIEX instruments, Framingham, MA, USA). The overall average recoveries from actual samples fortified with 22 antibiotics at three levels ranged from 73.8% to 98.5% based on the use of matrix-fortified calibration, with variations ranging from 5.80 to 12.4% (n= 6). The limits of detection and quantification were 0.3 μg kg−1and 1.0 μg kg−1, respectively. Lastly, the modified method was applied to practical sample analysis in the daily risk monitoring and assessment of food safety with satisfactory stability and robustness.Keywords:antibiotics residue;response surface methodology (RSM);quinolones;tetracyclines;multiple reaction monitoring (MRM)
研究领域:
分析化学
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食品科学
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药理学
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DOI
高影响因子
危险品化学品经营许可证（带存储）