衍生化-气相色谱-三重四极杆质谱法同时测定粮食作物中三氯甲基吡啶及其代谢物残留

建立了粮食作物中三氯甲基吡啶及其代谢物6-氯吡啶甲酸的衍生化-气相色谱-三重四极杆质谱(GC-MS/MS)检测方法。选取高粱、小麦、玉米及爆谷等典型的粮食作物,采用酸性乙腈提取,以浓硫酸作为三氯甲基吡啶代谢物的衍生化试剂,优化了衍生化反应的最佳反应条件,并使用GC-MS/MS分析,以内标法对三氯甲基吡啶及其代谢物进行定量检测。结果表明,在0.025～0.4 mg/L范围内,线性关系良好,相关系数(r²)均大于0.995,在3个不同添加水平下的平均回收率在80.4%～98.4%之间,相对标准偏差(RSD)在1.0%～10.1%之间。该方法操作简单、高效,灵敏度高,抗干扰能力强,回收率和重复性良好,能够满足粮食作物中三氯甲基吡啶及其代谢产物残留量的检测要求。

Simultaneous determination of nitrapyrin and its metabolite residues in food crops by derivatization with gas chromatography-triple quadrupole mass spectrometry

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 (n=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% (n=6). This new method satisfies the related regulations for the determination of nitrapyrin and its metabolite in crops.