气相色谱-三重四极杆质谱法快速测定糙米中氟虫腈及其代谢物残留

Rapid determination of fipronil and metabolites residue in unpolished rice by gas chromatography-triple quadrupole mass spectrometry

中文关键词:  气相色谱-三重四极杆质谱法  糙米  氟虫腈及其代谢产物  残留

英文关键词:gas chromatography-triple quadrupole mass spectrometry  unpolished rice  fipronil and its metabolites  residue

中文摘要:

      目的 建立气相色谱-三重四极杆质谱(gas chromatography-triple quadrupole mass spectrometry, GC-MS/MS)测定糙米中氟虫腈及其代谢产物氟甲腈、氟虫腈砜、氟虫腈硫醚残留的的分析方法。方法 糙米加水涡旋混匀后乙腈提取, 通过N-丙基乙二胺(primary secondary amine, PSA)、C18粉末、石墨化炭黑(graphitized carbon black, GCB)粉末净化提取液, 气相色谱-三重四极杆质谱多重反应离子监测模式(multiple reaction monitoring, MRM)检测, 以外标法定量。结果 在1~50 μg/L范围下, 氟虫腈及其代谢物具有良好的线性关系, 相关系数(r)均大于0.99, 在2、10、20 μg/kg 3个添加水平下, 氟虫腈及其代谢物的平均回收率为91.6%~109.9%, 相对标准偏差(relative standard deviation, RSD)为4.3%~6.3%。氟虫腈及其代谢物在糙米中的定量限为0.2~0.5 μg/kg, 定量限添加回收率在85.0%～108.0%, RSD为5.9%~6.9%。结论 该方法操作简单快速、试剂耗材消耗少、灵敏度高, 适用于快速处理大批量糙米中氟虫腈及其代谢产物的残留量检测。

英文摘要:

      Objective To establish an analytical method for the determination of fipronil and its metabolites of fipronil-desulfinyl, fipronil-sulfide and fipronil-sulfone residues in unpolished rice by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). Methods Unpolished rice was extracted by acetonitrile mixed with water vortex, cleaned up by primary secondary amine(PSA), C18 and graphitized carbon black(GCB), detected by gas chromatography-triple four-step mass spectrometry and multiple reaction monitoring(MRM), and quantified by external standard method. Results That calibration curve was linear in the range of 150 μg/L, and the correlation coefficients (r) were all higher than 0.99. When the spiked levels were 2, 10, 20 μg/kg, the average recoveries of fipronil and its metabolites were between 91.6%-109.9%, the relative standard deviations (RSD) were 4.3%6.3%. The limits of detection for fipronil and its metabolites in unpolished rice were 0.2-0.5 μg/kg. Quantitative limit addition the average recoveries of fipronil and its metabolites were between 85.0%-108.0%, the relative standard deviations were 5.9%6.9%. Conclusion This method is simple and fast to operate, consumes less consumables and has high sensitivity, and is suitable for quickly processing the residues of fipronil and its metabolites in large quantities of unpolished rice.