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建立了茶叶中氟虫腈残留量快速测定的气相色谱-电子轰击源质谱法。茶叶中的氟虫腈用正己烷-丙酮(7:3,V/V)混合液提取,经石墨化碳黑固相萃取小柱净化后,用正己烷-丙酮(9:1,V/V)混合液洗脱,浓缩定容后,用气相色谱-电子轰击源质谱法测定,外标法定量。结果表明,目标物质在0.001~0.040 mg/L范围内的线性关系良好;空白样品在0.002~0.010 mg/L范围三水平加标回收实验的平均回收率在96.6%~114.2%之间,相对标准偏差(n=6)为2.9%~4.4%;方法的定量限为0.001 mg/kg。该方法能满足茶叶中氟虫腈残留量0.002 mg/kg的检测要求。
The rapid determination of fipronil in tea by gas chromatography-electron impact mass spectrometry was established. Fipronil in tea was extracted with a mixture of n-hexane and acetone (7: 3, V / V) and purified with carbon black solid-phase extraction cartridges and eluted with n-hexane- ) Mixture eluting, concentrated to volume after determination by gas chromatography - electron impact mass spectrometry, external standard method. The results showed that the linearity of the target substance in the range of 0.001-0.040 mg / L was good. The average recoveries of three spiked samples in the range of 0.002-0.010 mg / L were between 96.6% and 114.2%. The relative standard Deviations (n = 6) ranged from 2.9% to 4.4%; the limit of quantification for the method was 0.001 mg / kg. The method can meet the detection requirement of 0.002 mg / kg of fipronil in tea.