Sun Linghui, Chen Jie, Xu Juan, Li Minqing, Chen Wenrui
Guangzhou Customs Technical Center, Key Laboratory of Animals and Plants and Food Import and Export of Technical Measures in Guangdong Province, Guangzhou 510623, China.
Se Pu. 2020 Jun 8;38(6):695-701. doi: 10.3724/SP.J.1123.2019.11030.
A method based on precolumn derivatization along with gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) was developed for the determination of nitrapyrin and its metabolite, 6-chloropicolinic acid, in crops. The samples were extracted by acid acetonitrile, and subjected to precolumn derivatization using a sulfoacid. The quantification of the analytes was performed by the internal standard method. Good linear relationships between the peak areas and mass concentrations of the analytes were obtained in the range of 0.025-0.2 mg/L with correlation coefficients greater than 0.995 (=6). The limits of quantification (LOQs) were 0.05 mg/kg. The recoveries of the analytes in crops at three spiked levels (0.05, 0.1, and 0.2 mg/kg) were in the range of 80.4%-98.4%, with relative standard deviations between 1.0% and 10.1% (=6). This new method satisfies the related regulations for the determination of nitrapyrin and its metabolite in crops.
建立了一种基于柱前衍生化结合气相色谱-三重四极杆质谱法（GC-MS/MS）测定作物中硝吡咯及其代谢物6-氯吡啶甲酸的方法。样品用酸性乙腈萃取，并用磺酸进行柱前衍生化。采用内标法对分析物进行定量。分析物的峰面积与质量浓度在0.025 - 0.2 mg/L范围内呈良好的线性关系，相关系数大于0.995（n = 6）。定量限（LOQs）为0.05 mg/kg。在三个加标水平（0.05、0.1和0.2 mg/kg）下，作物中分析物的回收率在80.4% - 98.4%范围内，相对标准偏差在1.0% - 10.1%之间（n = 6）。该新方法符合作物中硝吡咯及其代谢物测定的相关规定。
