Validation and use of a fast sample preparation method and liquid chromatography–tandem mass spectrometry in analysis of ultra-trace levels of 98 organophosphorus pesticide and carbamate residues in a total diet study involving diversified food types

2010 ◽  
Vol 1217 (29) ◽  
pp. 4815-4824 ◽  
Author(s):  
Stephen W.C. Chung ◽  
Benny T.P. Chan
Keyword(s):  
Preparation Method ◽  
Organophosphorus Pesticide ◽  
Tandem Mass ◽  
Sample Preparation Method ◽  
Total Diet Study ◽  
Chromatography Tandem Mass Spectrometry ◽  
Total Diet ◽  
Liquid Chromatography Tandem Mass ◽  
Diet Study ◽  
Ultra Trace

scholarly journals Simultaneous Analysis of Fenpropimorph and Fenpropimorph Acid in Six Different Livestock Products Using a Single-Sample Preparation Method Followed by Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2021 ◽  
Vol 26 (19) ◽  
pp. 5791
Author(s):  
Seon Wook Kim ◽  
Da Jung Lim ◽  
In Seon Kim
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
Tandem Mass Spectrometry ◽  
Preparation Method ◽  
Tandem Mass ◽  
Sample Preparation Method ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Livestock Products

Pesticides in livestock products must be measured to ensure food safety. We developed a single-sample preparation method followed by liquid chromatography–tandem mass spectrometry (LC-MS/MS) for simultaneous determination of fenpropimorph and fenpropimorph acid in six different livestock products. The extraction method was a modification of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and was validated according to the CODEX guidelines. The matrix-matched calibration curves for fenpropimorph and fenpropimorph acid exhibited good linearity, with coefficients of determination (R2 values) higher than 0.998. The limit of detection (LOD) and the limit of quantitation (LOQ) were 1.25 and 5.0 µg kg−1, respectively. The average recovery values ranged from 61.5% to 97.1% for samples fortified to the LOQ, 2 × LOQ, and 10 × LOQ. The method fully complied with the CODEX guidelines and was successfully applied to real samples obtained from domestic markets.

Analytical Method of Multi-Mycotoxins in Table-Ready Foods for a Total Diet Study Using Stable Isotope Dilution Liquid Chromatography–Tandem Mass Spectrometry

2019 ◽  
Vol 102 (6) ◽  
pp. 1657-1665
Author(s):  
Youngsun Lee ◽  
Jung Hee Kim ◽  
Da-Jung You ◽  
Cho-Il Kim ◽  
Jee-Yeon Lee ◽  
...  
Keyword(s):  
Stable Isotope ◽  
Isotope Dilution ◽  
Total Diet Study ◽  
Stable Isotope Dilution ◽  
Total Diet ◽  
Liquid Chromatography Tandem Mass ◽  
Diet Study ◽  
Mycotoxin Analysis ◽  
Raw Foods ◽  
Interlaboratory Reproducibility

Abstract Background: Determining the multi-mycotoxins present in table-ready foods is necessary for a total diet study. However, so far, most methods of analyzing multi-mycotoxins apply to raw foods. Therefore, a reliable method for analyzing multi-mycotoxins in table-ready foods is needed. Objective: We developed and validated methods of multi-mycotoxin analysis that employed stable isotope dilution with LC–tandem MS (LC–MS/MS) using two representative matrices. Methods: Samples were fortified with [13C]-labeled mycotoxins as internal standards and extracted with 50% acetonitrile in water for high-carbohydrate foods and 3% formic acid in acetonitrile for high-protein and/or high-fat foods, cleaned up with n-hexane and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, and followed up by LC–MS/MS. Results: Validation of the methods was performed, and the results were as follows: the correlation coefficient, R2, was 0.99; method detection limit, 0.01–2.4 μg/kg; recoveries, 83.6–114%; precision, 0.8–10 (intraday) and 3.1–22% (interday); interlaboratory reproducibility, ≤15%; and uncertainty, 3.5–19%error. The applicability of the methods was evaluated by analyzing table-ready foods spiked with standards. Conclusions: These methods were successfully evaluated and deemed appropriate for determining the multi-mycotoxins in table-ready foods. Highlights: This work demonstrates that stable isotope dilution with LC–MS/MS can be effectively used to analyze multi-mycotoxins simultaneously in a total diet study.

Analytical Method of Multi-Mycotoxins in Table-Ready Foods for a Total Diet Study Using Stable Isotope Dilution Liquid Chromatography–Tandem Mass Spectrometry

2019 ◽  
Vol 102 (6) ◽  
pp. 1657-1665
Author(s):  
Youngsun Lee ◽  
Jung Hee Kim ◽  
Da-Jung You ◽  
Cho-Il Kim ◽  
Jee-Yeon Lee ◽  
...  
Keyword(s):  
Stable Isotope ◽  
Isotope Dilution ◽  
Total Diet Study ◽  
Stable Isotope Dilution ◽  
Total Diet ◽  
Liquid Chromatography Tandem Mass ◽  
Diet Study ◽  
Mycotoxin Analysis ◽  
Raw Foods ◽  
Interlaboratory Reproducibility

Background: Determining the multi-mycotoxins present in table-ready foods is necessary for a total diet study. However, so far, most methods of analyzing multi-mycotoxins apply to raw foods. Therefore, a reliable method for analyzing multi-mycotoxins in table-ready foods is needed. Objective: We developed and validated methods of multi-mycotoxin analysis that employed stable isotope dilution with LC–tandem MS (LC–MS/MS) using two representative matrices. Methods: Samples were fortified with [13C]-labeled mycotoxins as internal standards and extracted with 50% acetonitrile in water for high-carbohydrate foods and 3% formic acid in acetonitrile for high-protein and/or high-fat foods, cleaned up with n-hexane and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, and followed up by LC–MS/MS. Results: Validation of the methods was performed, and the results were as follows: the correlation coefficient, R2, was 0.99; method detection limit, 0.01–2.4 μg/kg; recoveries, 83.6–114%; precision, 0.8–10 (intraday) and 3.1–22% (interday); interlaboratory reproducibility, ≤15%; and uncertainty, 3.5–19%error. The applicability of the methods was evaluated by analyzing table-ready foods spiked with standards. Conclusions: These methods were successfully evaluated and deemed appropriate for determining the multi-mycotoxins in table-ready foods. Highlights: This work demonstrates that stable isotope dilution with LC–MS/MS can be effectively used to analyze multi-mycotoxins simultaneously in a total diet study.

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