乳品中氨基甲酸酯类农药多残留高效液相色谱分析方法的研究

建立了乳品中氨基甲酸酯类农药（ＮＭＣＳ）多残留高效液相色谱（ＨＰＬＣ）紫外检测（ＵＶ）分析方法。采用ＯＤＳ色谱柱，确定甲醇－水（４５５５）为流动相，２１０ｎｍ下进行检测，速灭威、西维因、异丙威、呋喃丹、涕灭威等５种ＮＭＣｓ达到很好分离，分离度达２．２３以上。５种ＮＭＣｓ最低检测限为０．７５～３ｎｇ，标准曲线线性良好（ｒ＝０．９９４４～０．９９６３）。样品以丙酮提取，加入ＮａＣｌ使其饱和，再加入二氯甲烷分配，提取和分离农药一步完成。提取液再用交联聚苯乙烯凝胶（Ｂｉｏ－ＢｅａｄｓＳ－Ｘ３）净化。洗脱液为乙酸乙酯－环己烷（１１），收集流分为３５～６５ｍｌ，５种ＮＭＣｓ平均过柱回收率８６．８％～１００．０％。净化效果良好，样品添加５种ＮＭＣｓ的平均回收率在８０％以上，符合农药残留痕量分析要求。

Study on the Determination of N methylcarbamate Insecticides in Milk by HPLC

A high performance liquid chromatographic (HPLC) method using ultraviolet detector (210nm) for simultaneous determination of 5 carbamate insecticides in milk has been developed. Five carbamate insecticides aldicarb, MTMC, carbofuran, carbaryl and MIPC were separated on a reverse phase column (ODS) using methanol-water (45:55) mobile phase, and the resolution was higher than 2.23. The linearity for NMCs standards was good (r = 0.9944-0.9963) and the detection limits of 5 carbamate insecticides were 0.75-3.00 ng. Samples of milk were extracted with acetone. The extraction and partition were combined into one step by saturating the extraction solvent with NaCl and at the same time driving away the water by dichloromethane. The extract was cleaned up by gel permeation (Bio-Beads S-X3). The conditions of Bio-Beads S-X3 column for NMCs multiresidues analysis were studied. The elution solvent was ethyl acetate-cyclohexane (1: 1). The average recoveries of 5 NMCs in samples of milk were above 80%.