PRiME HLB固相萃取结合气相色谱-串联质谱法快速测定酸笋、酸豆角中氟虫腈及其代谢物残留量

Rapid determination of fipronil and its metabolites residues in fermented bamboo shoots and pickled cowpeas by PRiME HLB solid phase extraction combined with gas chromatography-tandem mass spectrometry

目的建立PRiMEHLB固相萃取结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)快速测定酸笋、酸豆角中氟虫腈及其代谢物残留量的分析方法。方法称取5g样品(酸笋、酸豆角),加入10 mL乙酸乙酯及6 g氯化钠振荡提取1 min,离心后取3 mL上清液经PRiME HLB通过式固相萃取柱净化,残留量采用气相色谱-串联质谱法进行检测。结果本研究建立的氟虫腈及其代谢物残留测定方法,在0.5~10.0 ng/mL线性范围内,相关系数(r^(2))均大于0.9994, 4种农药分析物在各自浓度范围内均呈现良好线性关系,方法定量限均为1.0μg/kg。在酸笋、酸豆角中加入低、中、高3个添加水平进行回收实验,平均回收率及相对标准偏差分别为91.7%~100.2%、0.7%~10.2%。结论该方法操作便捷、高效、环境友好,适合于酸笋、酸豆角中氟虫腈及其代谢物残留量的筛查。

Objective To establish a method for the rapid determination of fipronil and its metabolites residues in fermented bamboo shoots and pickled cowpeas by PRiME HLB solid phase extraction combined with gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods The 5 g samples(fermented bamboo shoots and pickled cowpeas) were weighed,mixed with 10 mL ethyl acetate and 6 g sodium chloride,shaken and extracted for 1 min,and then centrifugated.The 3 mL of supernatant was purified through PRiME HLB solid-phase extraction column.The residues were determined by gas chromatography-tandem mass spectrometry.Results In the linear range of 0.5-10.0 ng/mL,the correlation coefficients(r^(2)) of the method for the determination of fipronil and its metabolites residues established in this study were greater than 0.9994.The 4 kinds of pesticide analytes showed good linear relationship in their respective concentration range,and the limits of quantification of the method were 1.0 μg/kg.The recovery experiment was carried out by adding 3 addition levels of low,medium and high to fermented bamboo shoots and pickled cowpeas,the average recoveries and relative standard deviations were 91.7%-100.2% and 0.7%-10.2%,respectively.Conclusion This method is convenient,efficient and environment-friendly,and it is suitable for screening the residues of fipronil and its metabolites in fermented bamboo shoots and pickled cowpeas.