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目的建立气相色谱-串联质谱法同时测定花生油中250种农药残留的分析方法。方法样品经酸化乙腈提取,以乙腈+甲苯(3:1,V:V)作为洗脱液经C_(18)固相萃取柱净化,采用DB-5MS毛细管色谱柱分离;质谱采用电子轰击离子源模式电离,多反应监测模式对样品进行测定。结果本方法分为7组,完成250种目标化合物的分离分析。250种农药残留在0.02~0.2 mg/L范围内呈现良好的线性关系,相关系数r为0.990~0.999;样品中添加5、10和20μg/kg 3个浓度水平的250种农药混标工作液进行加标回收试验,平均回收率为70%~130%,RSD为1.8%~8.9%(n=5),检出限为5~10μg/kg。结论该方法准确、灵敏、重现性好、高通量,适合测定花生油中的多种农药残留。
Objective To establish a method for the simultaneous determination of 250 pesticide residues in peanut oil by gas chromatography-tandem mass spectrometry. Methods The samples were extracted with acidified acetonitrile and purified by C18 column with acetonitrile + toluene (3: 1, V: V) as eluent. The separation was performed on a DB-5MS capillary column. Mode ionization, multiple reaction monitoring mode for the determination of the sample. Results The method was divided into 7 groups to complete the separation and analysis of 250 target compounds. 250 kinds of pesticide residues in the range of 0.02 ~ 0.2 mg / L showed a good linear relationship, the correlation coefficient r was 0.990 ~ 0.999; samples were added at 5, 10 and 20μg / kg concentration of 250 pesticide mixed standard working solution The spiked recovery test showed that the average recovery was 70% ~ 130%, RSD was 1.8% ~ 8.9% (n = 5), and the detection limit was 5 ~ 10μg / kg. Conclusion The method is accurate, sensitive, reproducible and high-throughput and suitable for determination of a variety of pesticide residues in peanut oil.