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

中文关键词:  PRiME HLB  气相色谱-串联质谱法  酸笋  酸豆角  氟虫腈及其代谢物

英文关键词:PRiME HLB  gas chromatography-tandem mass spectrometry  fermented bamboo shoots  pickled cowpeas  fipronil and its metabolites

中文摘要:

      目的 建立PRiME HLB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5 g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(r2)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1.0 μg/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。

英文摘要:

      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 (r2) 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.