MOLECULES
·
2018
·Vol. 23
·期 8
·1926
·
IF 3.098
Bo Zhang,Xia Chen,Shun-Yu Han,Min Li,Teng-Zhen Ma,Wen-Jun Sheng,Xia Zhu
The aim of this study is to develop and validate an improved analytical method for the simultaneous quantification of 20 types of mycotoxins in grapes and wines. In this research, the optimization of tandem mass spectrometer (MS/MS) parameter, ultra-high pressure liquid chromatography (UHPLC) separation, and QuEChERS procedure, which includes wine/water ratio, the amount and type of salt, clean-up sorbent, were performed, and the whole separation of mycotoxins was accomplished within 7 min analyzing time. Under optimum conditions, recoveries ranged from 85.6% to 117.8%, while relative standard deviation (RSD) remained between 6.0% and 17.5%. The limit of detection (LOD, 0.06–10 μg/L) and the limit of quantification (LOQ, 0.18–30 μg/L) were lower than those permitted by legislation in food matrices, which demonstrated the high sensitivity and applicability of this efficient method. Finally, 36 grapes and 42 wine samples from the Hexi Corridor region were analyzed. Penicillic acid (PCA), mycophenolic acid (MPA), cyclopiazonic acid (CPA), fumonisin B1 (FB1) and zearalenone (ZEN) were detected in a small number of grape samples with lower concentrations between 0.10 μg/L and 81.26 μg/L. Meanwhile, ochratoxin A (OTA), aflatoxin B2 (AFB2), MPA, CPA, and ZEN were detected in some wine counterparts with concentrations ranged from 0.10 μg/L to 4.62 μg/L. However, the concentrations of the detected mycotoxins were much lower than the maximum legal limits set of other products.Keywords:QuEChERS;UHPLC–MS/MS;mycotoxins;grapes and wines;hexi corridor region
研究领域:
食品科学
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分析化学
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农业化学
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产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2020
·Vol. 25
·期 9
·2149
·
IF 3.267
Xu Yu,Fei Ma,Liangxiao Zhang,Peiwu Li
Rapeseed (Brassica napus L.) is rich in phenols, vitamins, carotenoids, and mineral elements, such as selenium. Additionally, it contains the active ingredients sulforaphane and indole-3-carbinol, which have been demonstrated to have pharmacological effects. In this study, sulforaphane and indole-3-carbinol were extracted and quantified from rapeseeds using quick, easy, cheap, effective, rugged and safe (QuEChERS) method coupled with ultra high performance liquid chromarography tandem mass spectrometry (UHPLC-MS/MS). The major parameters for extraction and purification efficiency were optimized, including the hydrolysis reaction, extraction condition and type and amount of purification adsorbents. The limit of detection (LOD) and the limit of quantification (LOQ) for sulforaphane were 0.05 μg/kg and 0.15 μg/kg, and for indole-3-carbinol were 5 μg/kg and 15 μg/kg, respectively. The developed method was used to successfully analyze fifty rapeseed samples. The QuEChERS coupled with UHPLC-MS/MS simultaneously detect sulforaphane and indole-3-carbinol in vegetable matrix and evaluate the quality and nutrition of rapeseed samples.Keywords:sulforaphane;indole-3-carbinol;QuEChERS;quantification;UHPLC-MS/MS
研究领域:
农业化学
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分析化学
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食品科学
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产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2016
·Vol. 8
·期 19
·3953-3958
·
IF 1.915
Zhiqing Xun,Jinfeng Huang,Xiu-Ying Li,Senyu Lin,Shuang He,Xindong Guo,Yanping Xian
By utilizing gas chromatography tandem mass spectrometry (GC/MS) and QuEChERS purification technology, a new method was developed for the detection of seven acrylate compounds (methyl methacrylate, butyl acrylate, sec-butyl acrylate, 2-ethylhexyl acrylate, glycidyl methacrylate, n-octyl acrylate, and N-octyl methacrylate) in food contact paper products. Hexane was used as the extraction solvent and carbon nanotubes were used as adsorbents during the QuEChERS purification. The acrylates were separated by an ultra-inert column (DB-5MS UI) and detected in the electron ionization mode of MS with selected ions monitoring (SIM). Under the optimal conditions, the calibration curves for the seven analytes were linear in the range of 5.0–1000 μg L−1 with the correlation coefficients higher than 0.9984. The quantitation limits of the method (S/N = 10) of these acrylates were in the range of 50.0–100.0 μg kg−1. The mean recoveries for paper products at three spiked concentration levels of 50.0–1000 μg kg−1 were in the range of 82.1–106.5%, and the relative standard deviations (RSDs, n = 6) ranged from 1.5% to 5.6%. This method is accurate, simple and rapid, and could be applied to the detection of acrylates in food contact paper products.
研究领域:
分析化学
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食品安全
✓ 已验证
产品关联
DOI
高影响因子
ANALYTICAL SCIENCES
·
2023
·Vol. 39
·期 7
·1151-1161
·
IF 1.6
Zhang Zhihui,Zhang Jingyu,Li Mufei,Jin Xiangzi,Yao Liping,Wang Wenyuan,Liu Jinsong,Li Zuguang
This work first proposed a novel green and efficient method based on Quick, Easy, Cheap, Efficient, Rugged, and Safe pretreatment (QuEChERS) combined with switchable hydrophilic solvent homogeneous liquid–liquid microextraction (SHS-HLLME) for trace determination of triazole fungicides (TFs) in agricultural products such as vegetables and fruits by gas chromatography–mass spectrometry (GC–MS). N , N -Dimethyl benzylamine was used for the synthesis of SHS. Box–Behnken design was applied for the optimization of extraction conditions and a mathematical model was obtained. Ultimately, 0.50 mL SHS, 1.0 mL 10 mol L −1 sodium hydroxide, and 45 s ultrasonic time were determined as optimal conditions for the SHS-HLLME method. The limit of detection and limit of quantification determined using the optimal method (SHS-HLLME/GC–MS) were 0.13–0.27 ng mL −1 and 0.43–0.90 ng mL −1 , respectively. In addition, the SHS-HLLME method under optimal conditions was combined with the traditional QuEChERS method to realize the advancement of the SHS-HLLME method from simple to complex matrix analysis, and the QuEChERS–SHS-HLLME method was successfully applied to the analysis of TFs in cucumbers, tomatoes, watermelon and grapes in agricultural products. Matrix-matched calibration standards were used to improve the accuracy of TFs in spiked cucumber samples to obtain recovery results close to 100%. It was shown that the new method is green and rapid, enabling fast and inexpensive sample pretreatment with up to 100-fold enrichment factor and low detection limit compared with the original QuEChERS method. Graphical abstract
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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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Qi Zhou,Lihong Wang,Canping Pan,Congcong Yu,Jin Hua,Tao Lan
Considering the matrix characteristics of honeysuckle and chrysanthemum, a comprehensive and systematic extraction and purification processes study for pesticide residue analysis in these two Traditional Chinese Medicine (TCM) were conducted based on a nanomaterial-modified QuEChERS method. For honeysuckle, a combination of 60 mg FeN-MWCNTs and 60 mg PSA provided the best purification effect. For chrysanthemum, 70 mg GCB and 30 mg PSA achieved the optimal results. Our initial exploration into the purification mechanism of the nanomaterials revealed that micropores and smaller mesopores in the adsorbents play a crucial role, while amino groups primarily govern the adsorption process, with matrix impurities adhering to the surface of the nano-adsorbents. The limit of quantification (LOQ) for honeysuckle in this method ranged from 0.12 to 18.86 µg/kg, with recovery rates between 60.1 % and 128.6 %, and relative standard deviations (RSD) less than 12 %. For chrysanthemum, the LOQ was between 0.10 and 8.56 µg/kg, and the recovery rates for 27 pesticides were in the range of 61.6 % to 118.9 %. Applying this method, 105 honeysuckle and 111 chrysanthemum market samples were analyzed, detecting five pesticides in 18 honeysuckle and 12 chrysanthemum samples respectively. This study offers a targeted strategy for the development of analytical methods for trace substances in complex matrices.
研究领域:
分析化学
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中药学
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环境科学
✓ 已验证
产品关联
DOI
高影响因子
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2023
·Vol. 37
·期 13
·e9518
·
IF 2
Lihua Qu,Xiaoyu Qi,Li Zhao,Yu Zhang,Ronghua Zhuge,Zhihui Hao,Congmin Liu
Rationale The residues of fipronil and its metabolites in chicken eggs pose a threat to human health, so regular monitoring is necessary. However, the pretreatments of the existing detection methods are complex and time-consuming. A simple and streamlined pretreatment method is needed to improve the detection efficiency. Method A rapid, efficient, and facile approach employing the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method with online solid-phase extraction liquid chromatography tandem Q Exactive Orbitrap high-resolution mass spectrometry (online-SPE-LC-HRMS) was established and evaluated for the determination of fipronil, fipronil-desulfinyl, fipronil-sulfone, and fipronil-sulfide in chicken eggs. An improved sample preparation technique combining QuEChERS and online-SPE was developed. Negative targeted ion fragmentation scanning and targeted-selected ion monitoring of HRMS were adopted to identify and quantify the target analytes. Results The proposed pretreatment method took a few steps in <13 min to achieve excellent recoveries and negligible interference. High selectivity was acquired with the adoption of Q/Orbitrap HRMS. The limit of quantification (LOQ) of the analytes was 2.5 μg kg −1 , meeting the detection requirements of the maximum residue level enacted by the Codex Alimentarius Commission, Japan, and the United States for the sum of fipronil and its metabolites. Extraction recoveries at three spiked concentration levels were within 84.56% to 93.84%, with relative standard deviation ≤5.87%. Conclusion The established method is efficient and easy to operate and displays satisfactory LOQs, recoveries, accuracy, and precision. This approach serves as a reference method for monitoring eggs while providing potential solutions for fipronil determination in more complicated matrices.
研究领域:
食品安全
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分析化学
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毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CONTROL
·
2024
·
IF 5.6
Luyao Zhao,Jin Liu,Bing Bai,Yongpeng An,Yukun Yang,Xiaowen Wang,Xu Jing
Herein, we established a green, rapid, and sensitive method to analyze ochratoxin A (OTA) in cereals based on modified QuEChERS and enzyme-linked immunosorbent assay (ELISA). Lignocellulose is a renewable material mainly consisting of cellulose, hemicellulose, and lignin. In the modified QuEChERS, a natural deep eutectic solvent synthesized from glucose and levulinic acid derived from cellulose and hemicellulose was used as an extraction solvent to replace traditional organic solvents. Furthermore, modified lignin was used as an adsorbent to purify the extraction solution. In the magnetic bead-based ELISA, the effervescent reaction accelerated the immune competition. Additionally, magnetic beads were used to shorten the incubation and washing time, whereas gold nanoparticles were used to amplify the optical signal. This method has been successfully applied to the analysis of OTA in cereal samples. The limits of detection were 0.68–0.83 μg kg −1 . This pretreatment and detection strategy has potential application in analyzing mycotoxins.
研究领域:
食品安全
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分析化学
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生物技术
✓ 已验证
产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2020
·
IF 6.306
Congcong Yu,Dongyu Hao,Qiao Chu,Ting Wang,Songnan Liu,Tao Lan,Fenghe Wang,Canping Pan
Tea polyphenols, chlorophyll and lutein generally cause strong matrix effects and challenge analysis of trace substances in tea. Seven frequently used adsorbents were chosen to test removal ability for tea polyphenols, chlorophyll and lutein based on the adsorption isotherm fitting. Results showed that MWCNTs-NH 2 demonstrated the strongest removal ability, which may be ascribed to the π-π and electrostatic interaction. Then a method of MWCNTs-NH 2 modified QuEChERS coupled with HPLC-MS/MS detection of 10 organophosphorus pesticide residues in tea was developed and validated. Unlike traditional QuEChERS, only one adsorbent (MWCNTs-NH 2 ) was applied in this method to replace the combined effect of various adsorbents, which improved the easiness and generality of the method. The LOQs were 1.7–9.0 µg/kg. The average recovery rate ranged from 72% to 116% with RSDs less than 14%. This study provides a targeted strategy to develop analysis method for trace substances in a complicated matrix.
研究领域:
分析化学
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食品科学
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2016
·
IF 2.687
Hongcheng Liu,Tao Lin,Xianglei Cheng,Ning Li,Luxiang Wang,Qiwan Li
A simple, accurate and highly sensitive multiresidues method was developed for the determination of 9 anabolic steroids and 16 β-agonists in milk. Target compounds were extracted and separated by a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) method with Primary secondary amine (PSA) and Zinc oxide (ZnO) nanoparticles as adsorbents. The analytes were determined by ultra high performance liquid chromatography coupled to an electro-spray ionization tandem mass spectrometer (UHPLC–MS/MS) operating in negative/positive multiple reaction monitoring mode. The effect of QuEChERS including organic solvent, amount of ZnO nanoparticle was evaluated. Good linearity was obtained for the analytes in the concentration range of 0.1–200 μg/L with a correlation coefficients higher than 0.994. Decision limits (CCα) was from 0.007 μg/kg–0.1 μg/kg, and detection capabilities (CCβ) was in the range of 0.02–0.4 μg/kg. The recoveries of these compounds were between 63% and 126% at three fortified levels. Reproducibility represented by RSD was with 10% or less. The method was successfully applied to screening of real milk samples obtained from local markets and confirmation of the suspected target analytes.
研究领域:
食品科学
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分析化学
✓ 已验证
DOI
高影响因子
ANALYTICAL LETTERS
·
2024
·
IF 1.6
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.
研究领域:
分析化学
·
食品安全
✓ 已验证
产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2018
·
IF 4.946
Chunjian Wu,Li Wang,He Li,Shujuan Yu
The determination of carcinogenic 4(5)-methylimidazole (4-MeI) in complex matrices at trace levels is a challenge because of its higher polarity and weaker column retention capability. Here, we proposed a novel method for the quantification of 4-MeI in various foods and beverages using modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction with liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. The evaluated QuEChERS extraction with LC-MS/MS method showed excellent linearity (1–200 μg/L, with correlation coefficient (R 2 ) > 0.999), trueness (91–113%), and precision (relative standard deviation (RSD) ≤ 12.3%), but low matrix effect (92–108%) for cola, tea, beer, coffee beverage, bread, biscuit and instant coffee. The expanded measurement uncertainty was less than 34.4% at 95% confidence level. The proposed method can be successfully applied to determine 4-MeI in 28 commercial foods and beverages purchased from local market. Therefore, we believe this method is likely to provide a potential for 4-MeI determination in practical application.
研究领域:
分析化学
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食品安全
·
毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Journal of Analysis and Testing
·
2022
·Vol. 7
·期 2
·163-171
·
IF 0
Qu Gang,Chen Bo,Liu Shilei,Zhang Qiaoli,Yang Yang,Fu Qingshan
Organophosphate nerve agents (OPNAs) are lethal chemical weapons (CWs) which hydrolyze rapidly to alkyl phosphate compounds in the environment. The identification of alkyl phosphate compounds in the environment is critical for the verification of OPNAs. Currently, due to the complex sample preparation and long detection process for organophosphate nerve agent hydrolysis products (OPNAHPs), their high-throughput determination is difficult. To simplify sample preparation and detection of OPNAHPs from environmental samples, a quick, easy, cheap, effective, rugged and safe (QuEChERS) method for the simultaneous purification of the five OPNAHPs in environmental samples combined with detection through direct analysis in real-time ionization source coupled with tandem mass spectrometer (DART-MS/MS) was developed. An internal standard method was applied for the quantification. The method exhibited a good linearity ( R 2 > 0.991) in the range of 1.00 ng/mL-4.00 μg/mL. The limits of detection and limits of quantification were 1.00–7.00 ng/mL and 10.0–20.0 ng/mL, respectively. The recoveries of OPNAHPs in environmental samples were between 65.3% and 107%, with relative standard deviations ranged from 1.6% to 19%. In addition, the sample preparation and analysis process for OPNAHPs could be completed in less than 10 min. The results demonstrated that the modified QuEChERS method could quickly and efficiently remove the matrix of environmental samples. Combined with DART-MS/MS, an accurate and high-throughput detection method of OPNAHPs in environmental samples was provided. The developed method has great potential in the fields of early warning, clinical treatment and environmental decontamination.
研究领域:
分析化学
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环境科学
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毒理学
✓ 已验证
产品关联
DOI
危险品化学品经营许可证（带存储）