固相萃取-高效液相色谱-串联质谱法同时测定银耳中的8种农药残留

Determination of Eight Pesticide Residues in Tremella fuciformis Berk by Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了同时测定银耳中吡虫啉、啶虫脒、异丙威、丁硫克百威、克百威、甲胺磷、乙酰甲胺磷和咪鲜胺8种常见农药残留的固相萃取-高效液相色谱-串联质谱分析方法。5 g样品,加入1 g NaCl,用乙酸乙酯提取,提取液通过C18柱固相萃取净化后,以Phenomenex Luna C8色谱柱(150 mm×2.0 mm×3.0μm)分离,流动相A为含0.1%甲酸-5 mmol/L NH 4Ac溶液,流动相B为乙腈,梯度洗脱。质谱采用多反应监测(MRM)模式检测,外标法定量。结果显示:吡虫啉在1.0~1000.0μg/L,啶虫脒、异丙威、丁硫克百威、克百威和咪鲜胺在1.0~500.0μg/L,甲胺磷和乙酰甲胺磷在1.0~250.0μg/L范围内线性良好,相关系数(r 2)均大于0.995;检出限为0.01~0.30μg/kg,定量限为0.03~1.00μg/kg。在低、中、高3个水平加标的回收率为70.1%~106.4%,相对标准偏差(RSD)为3.97%~13.68%。实际样品检测结果表明该方法稳定、准确、可靠。

An analytical method was developed using high performance liquid chromatography-tandem mass spectrometry for detecting the residues of eight pesticides in Tremella fuciformis Berk.Eight pesticides in Tremella fuciformis Berk were extracted with ethyl acetate and purified with C18 solid-phase extraction cartridge.The pesticides were separated with a Phenomenex Luna C8(150 mm×2.0 mm×3.0μm)using(0.1% formic acid and 5 mmol/L ammonium acetate)-acetonitrile as mobile phase.Eight pesticides were analyzed by tandem mass spectrometry with external standard method under multiple reaction monitoring mode.The results showed that good linearity was obtained for imidacloprid at the mass concentrations of 1.0-1000.0μg/L,acetamiprid,isoprocarb,carbosulfan,carbofuran and prochloraz at the mass concentrations of 1.0-500.0μg/L,methamidophos and acephate at the mass concentrations of 1.0-250.0μg/L with the correlation coefficients higher than 0.995.The average recoveries of eight pesticides in Tremella fuciformis Berk at three spiked levels were in the range of 70.1%-106.4%,with relative standard deviations of 3.97%-13.68%.The limits of detection of eight pesticides were 0.01-0.30μg/kg.The limits of quantitation of eight pesticides were 0.03-1.00μg/kg.The proposed method was successfully applied in the detection of real samples with good repeatability.