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采用固相萃取净化前处理技术,结合气相色谱-串联质谱(GC-MS/MS)法建立了人参中11种农药同时检测的方法。样品用1%冰乙酸和乙腈的混合溶液提取,提取液离心后,上清液经填有无水硫酸镁、乙二胺-N-丙基硅烷(PSA)、十八烷基硅烷键合硅胶、硅胶和石墨化炭黑的固相萃取柱净化,浓缩、复溶后进行GC-MS/MS测定,采用多反应监测模式,内标法定量。当11种农药加标水平为0.004,0.01 mg/kg时回收率为54%~103%,方法的相对标准偏差小于15%;检出限(S/N=3)不高于6μg/kg;在10~1000μg/L范围内线性关系良好。方法适用于复杂基质中农药的多残留检测。
The method of simultaneous determination of 11 pesticides in Panax ginseng was established by GC-MS / MS method using solid phase extraction and pretreatment. The sample was extracted with a mixture of 1% glacial acetic acid and acetonitrile. After the extract was centrifuged, the supernatant was filled with anhydrous magnesium sulfate, ethylenediamine-N-propylsilane (PSA), octadecylsilane bonded silica , Silica gel and graphitized carbon black solid phase extraction column purification, concentration, reconstituted GC-MS / MS determination, the use of multi-reaction monitoring mode, internal standard method. When the spiked levels of 11 pesticides were 0.004,0.01 mg / kg, the recoveries were 54% -103%. The relative standard deviation of the method was less than 15%. The detection limit (S / N = 3) was not higher than 6μg / kg. The linearity was good in the range of 10 ~ 1000μg / L. The method is suitable for the detection of pesticide residues in complex matrices.