测定中药材中氨基甲酸酯类杀虫剂残留的高效液相色谱柱后衍生法

HPLC determination of residual carbamate insecticides in Chinese crude drugs post column derivation method

目的:采用高效液相色谱柱后衍生法测定中药材中氨基甲酸酯类杀虫剂残留。方法:通过乙腈提取,固相萃取(SPE)净化,Waters carbmate analysis(3.9mm×150min,4μm)柱,甲醇-水-乙腈(16:68:16)为流动相,柱温30℃,流速1.5mL·min^(-1)进行分离,柱后衍生反应系统,OPA 和氢氧化钠流速均为0.5mL·min^(-1),反应温度80℃,2475荧光检测器进行监测,进样20μL。结果:速灭威、克百威和西维因的添加回收率分别为84.6%～110.5%,86.9%～99.8%,90.1%～110.5%;RSD 分别为4.0%～8.6%,3.8%～8.5%,3.1～7.5%;最低检测限分别为0.01,0.01,0.005μg·mL^(-1)。结论:该方法分离效果好,灵敏度高。

Objective：To determine the residues of carbamate insecticides in Chinese crude drugs by HPLC -post column derivation. Method： The sample was extracted by acetonitrile, purified by Solid Phase Extract （ SPE）, separated with Waters carbmate analysis （3.9 mm ×150mm,4μm） ,methanol - water -acetonitrile（ 16： 68： 16）as mobile phase at column temperature of 30 ℃ and a flow rate of 1. 5 mL ·min^-1 and the system of post column deri- vation is a flow of OPA and NaOH （0. 5 mL ·min^-1 ） and the reaction is in the temperature of 80 ℃, detected with 2474 Fluorescence detector. Result ：The recoveries of tsumacide, carbofuran and carbaryl were 84. 6% - 110. 5%, 86. 9% -99. 8% ,90. 1% - 110. 5% ,respectively;Corresponding RSD were 4. 0% -8. 6% ,3.8% -8.5% ,3. 1 - 7.5% ,respectively. The detection limits were 0. 01 g ·mL^-1 ,0. 01 g ·mL^-1 and 0. 005 g ·mL^-1. Conclusion： The method is more selective and sensitive.