Development of an Analytical Method of Nereistoxin and Nereistoxin-related Pesticides in Agricultural Products by LC-MS/MS
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A simultaneous analytical method was developed for the quantification and confirmation of nereistoxin and nereistoxin-related pesticides in agricultural products. These pesticides were extracted with a 2% L-cysteine solution in 0.05 N HCI and hydrolyzed using ammonium hydoxide and 3% nickel(II) chloride solution, purified using dispersive solid phase extraction (d-SPE) kit, and then analyzed by LC-MS/MS. To prevent the matrix effect, all analytes were quantified using matrix-matched calibrations, as assessed by the determination coefficient (R2) of the range from 0.9951-1.000. The LOD and LOQ were satisfactory for determining low residual levels of the pesticides in agricultural products. The accuracy and precision of the method were evaluated based on recoveries with five replicates at three fortification levels (LOQ, 10×LOQ and 50×LOQ). The mean recoveries of nereistoxin and nereistoxin-related pesticides in agricultural products were 75.3-108.0% with a coefficient of variation of 0.8-7.0%. All the optimized results were excellent, as assessed by the Ministry of Food and Drug Safety guidelines and the Codex Alimentarius Commission guidelines for pesticide residue analysis. This study provides fundamental data for setting the residue definition and maximum residue limits for nereistoxin and nereistoxin-related pesticides in agricultural products.
Abstract
A simultaneous analytical method was developed for the quantification and confirmation of nereistoxin and nereistoxin-related pesticides in agricultural products. These pesticides were extracted with a 2% L-cysteine solution in 0.05 N HCI and hydrolyzed using ammonium hydoxide and 3% nickel(II) chloride solution, purified using dispersive solid phase extraction (d-SPE) kit, and then analyzed by LC-MS/MS. To prevent the matrix effect, all analytes were quantified using matrix-matched calibrations, as assessed by the determination coefficient (R2) of the range from 0.9951-1.000. The LOD and LOQ were satisfactory for determining low residual levels of the pesticides in agricultural products. The accuracy and precision of the method were evaluated based on recoveries with five replicates at three fortification levels (LOQ, 10×LOQ and 50×LOQ). The mean recoveries of nereistoxin and nereistoxin-related pesticides in agricultural products were 75.3-108.0% with a coefficient of variation of 0.8-7.0%. All the optimized results were excellent, as assessed by the Ministry of Food and Drug Safety guidelines and the Codex Alimentarius Commission guidelines for pesticide residue analysis. This study provides fundamental data for setting the residue definition and maximum residue limits for nereistoxin and nereistoxin-related pesticides in agricultural products.
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