scholarly journals Pesticide Residue Analysis of a Dietary Ingredient by Gas Chromatography/Selected-Ion Monitoring Mass Spectrometry Using Neutral Alumina Solid-Phase Extraction Cleanup

2008 ◽  
Vol 91 (3) ◽  
pp. 630-636 ◽  
Author(s):  
Mijeong Lee Jeong ◽  
Michael Zahn ◽  
Thao Trinh ◽  
Fay A Brooke ◽  
Wenwen Ma

Abstract A sample cleanup procedure has been developed to remove coextractives that interfere with pesticide residue analysis of a dietary ingredient (Product B), an extract consisting of Scutellaria baicalensis and Acacia catechu. Samples were extracted using 1 acetic acid in acetonitrile, followed by solid-phase extraction and analysis by capillary gas chromatography with mass spectrometry in the selective-ion monitoring mode. Neutral alumina (alumina N) was found to be the most effective sorbent to remove coextractives from Product B; other materials that were tested but failed to remove interference were graphitized carbon black/primary-secondary amine (PSA), octadecylsilane (C18), Florisil, Oasis MCX, and strong anion exchange-PSA. The method was specifically developed for Product B, which was spiked with 41 organochlorine and organophosphorus pesticides, and resulted in the recovery of 80 to 120 at U.S. Pharmacopeia limits (0.06 to 4 g/g) for the majority of the pesticides.

1991 ◽  
Vol 16 (2) ◽  
pp. 247-255 ◽  
Author(s):  
Yoshitsugu ODANAKA ◽  
Naomi TOMIYAMA ◽  
Yukiko KOMA ◽  
Osami MATANO ◽  
Shinko GOTO

Author(s):  
Peng Sun ◽  
Shusheng Zheng ◽  
Rui Yan ◽  
Yongfu Lian

Abstract In this study, a method was developed for determination of three organophosphorus pesticides (OPPs) using graphene aerogel solid-phase extraction (SPE) combined with gas chromatography–mass spectrometry (GC–MS). The experimental results showed that the target analytes could be extracted on packed SPE cartridges and then eluted with tetrahydrofuran. The final sample solution was analyzed by GC–MS, which demonstrated good linearity between 0.5 and 500 μg L−1 with a correlation coefficient (r) of 0.9991–0.9998. The limits of detection (S/N = 3) and the limits of quantification (S/N = 10) for the three OPPs ranged from 0.38 to 0.82 μg L−1 and 1.32 to 2.75 μg L−1, respectively. The accuracy of the proposed method was evaluated by measuring the recovery of the spiked samples, which ranged from 91.2 to 103.7%, with relative standard deviations of 2.1–7.2%. This method was successfully applied for the determination of the target analytes in water samples taken from tap, wetlands and canal water.


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