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建立了分散固相萃取-气相色谱测定对虾中12种有机磷农药残留的分析方法。样品经V(冰乙酸):V(乙腈)=1:99溶液提取,采用乙二胺-N-丙基硅烷(PSA)、C18与石墨炭黑(GCB)为吸附剂进行分散固相萃取净化。以DB-17毛细管色谱柱分离,GC-FPD(P)检测。方法在0.01~0.50μg/mL范围内线性关系良好,相关系数(r2)均不低于0.9971,12种有机磷农药的方法检出限均为0.01 mg/kg。在0.01~0.10 mg/kg的添加水平下,平均加标回收率为80.7%~101.2%,相对标准偏差为3.7%~7.6%。
A method for the determination of 12 organophosphorus pesticide residues in shrimp by dispersive solid-phase extraction and gas chromatography was established. The samples were extracted with V (acetonitrile) = 1: 99 by using V (acetonitrile) = 1: 99. The samples were purified by dispersive solid phase extraction using ethylenediamine-N-propylsilane (PSA), C18 and graphite carbon black . The separation was performed on a DB-17 capillary column and detected by GC-FPD (P). The method has a good linear relationship in the range of 0.01-0.50 μg / mL with the correlation coefficient (r2) no less than 0.9971. The detection limits of the 12 organophosphorus pesticides are both 0.01 mg / kg. Under the condition of 0.01-0.10 mg / kg, the average recovery was 80.7% ~ 101.2% with the relative standard deviation of 3.7% ~ 7.6%.