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目的建立一种多壁碳纳米管固相萃取净化-气相色谱质谱联用同时测定茶叶中26种农药的检测方法。方法样品经乙腈提取,过滤型多壁碳纳米管柱净化后,使用气相色谱质谱仪检测。结果碳纳米管净化能够有效去除茶叶中干扰物质,简化实验步骤,降低前处理过程中农药的分解。26种农药在0.04~1.6μg/m L范围内具有较好的线性。方法的检出限为0.005~0.05 mg/kg,定量下限为0.015~0.15 mg/kg。采用该方法对茶叶样品进行加标回收率实验,加标回收率在66.6%~125.5%,相对标准偏差为0.3%~6.4%(n=5)。结论该方法快速、准确、灵敏,适合茶叶中多种农药的同时测定。
OBJECTIVE To establish a method for the simultaneous determination of 26 pesticides in tea by multi-walled carbon nanotube solid phase extraction and gas chromatography-mass spectrometry. Methods The samples were extracted with acetonitrile and cleaned with a multi-walled carbon nanotube column. The samples were detected by gas chromatography-mass spectrometry. Results Carbon nanotube purification can effectively remove interfering substances in tea, simplify the experimental procedures and reduce the decomposition of pesticides in the pretreatment process. 26 kinds of pesticides in the 0.04 ~ 1.6μg / m L range with good linearity. The detection limit of this method was 0.005 ~ 0.05 mg / kg and the lower limit of quantitation was 0.015 ~ 0.15 mg / kg. The spiked recoveries of tea samples were tested by this method. The spiked recoveries ranged from 66.6% to 125.5% and the relative standard deviations (RSDs) ranged from 0.3% to 6.4% (n = 5). Conclusion The method is rapid, accurate and sensitive and suitable for the simultaneous determination of various pesticides in tea.