摘要
建立了分散固相萃取-液相色谱-电喷雾质谱联用方法定量检测土壤和甘蓝中虫酰肼残留量。应用分散固相萃取方法进行前处理,即以乙二胺-N-丙基硅烷(PSA)为吸附剂,乙腈为萃取溶剂,实现样品快速制备;在Zorbax Eclipse XDB-C18色谱柱上,以0.1%乙酸水-乙腈溶液(50/50,V/V)为流动相,采用电喷雾质谱检测器,选择离子监测模式,以m/z297为检测定量离子。虫酰肼保留时间在15min左右,线性范围为0.01～20μg·g-1,相关系数为0.9995,添加浓度为0.02,0.20,2.00mg·L-1时,土壤和甘蓝中虫酰肼的平均添加回收率在90.5%～103.0%之间,相对标准偏差(RSD,n=5)在1.2%～8.0%之间,最低检测浓度为0.02mg·kg-1。该方法灵敏、准确、可靠,定量范围宽,耐用性强,可作为土壤和甘蓝中虫酰肼残留的可靠检测方法。
A liquid chromatography-mass spectrometry （LC-MS） method was established for the determination of tebufenozide in soil and cabbage by dispersive solid phase extraction using acetonitrile as extraction solvent and primary secondary amine （PSA） as sorbent. The HPLC conditions：Zorbax Eclipse XDB-C18 column, 0.1% acetic acid acetonitrile solvent as mobile phase. Tebufenozide was detected in selected ion monitoring （SIM） mode with m/z 297 for quantification. Linear range was obtained between 0.01-20 μg·g^-1 with linear correlation coefficient of 0.999 5. The limit of quantification was 0.02 mg·kg^-1 for soil and cabbage. The mean recoveries were 90.5%-105% with relative standard deviations ranging from 1.2% to 8.0%. The results indicated that this method was sensitive, reliable and robust for the quantification of tebufenozide in soil and cabbage.
出处
《湖北农业科学》
北大核心
2009年第2期442-444,共3页
Hubei Agricultural Sciences
基金
湖北省农业科技创新中心资助项目(2007-620-001-03)
