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目的建立同时测定茶叶中溴虫腈和茚虫威的气相色谱-质谱联用(GCMS)检测方法。方法样品经乙腈均质,提取离心,提取液经CARB/NH2柱净化后,再经SLH小柱净化,以DB-5MS毛细柱(30 m×0.25 mm×0.25μm)分离后,在选择离子扫描模式(SIM)下进样分析,外标法定量。结果该法对于溴虫腈和茚虫威的线性范围均为0.10~10μg/m L,测定茶叶样品的检出限分别为0.01和0.008 mg/kg,定量限分别为0.03和0.025 mg/kg。加标回收率为75.6%~92.7%,相对标准偏差为3.6%~11.4%(n=6)。结论该法净化效果好,结果准确,适用于茶叶样品中溴虫腈和茚虫威的同时检测。
Objective To establish a gas chromatography-mass spectrometry (GC-MS) method for the simultaneous determination of chlorfenapyr and indoxacarb in tea. Methods The samples were homogenized with acetonitrile, extracted and centrifuged. The extracts were purified by CARB / NH2 column, then purified by SLH cartridge and separated by DB-5MS capillary column (30 m × 0.25 mm × 0.25 μm) Mode (SIM) under the injection analysis, external standard quantitative. Results The linear range of the method for chlorfenapyr and indoxacarb was 0.10-10 μg / mL. The detection limits of tea leaf samples were 0.01 and 0.008 mg / kg, respectively. The limits of quantification were 0.03 and 0.025 mg / kg, respectively. The spiked recoveries ranged from 75.6% to 92.7% with relative standard deviations of 3.6% to 11.4% (n = 6). Conclusion The method has good purification effect and accurate result. It is suitable for the simultaneous detection of chlorfenapyr and indoxacarb in tea samples.