中药材黄芪中农药残留量检测方法研究

Determination of Organochlorine Pesticide Residues in Astragalus

建立了中药黄芪中8种有机氯农药残留气相色谱分析方法。样品用石油醚-乙酸乙酯（体积比2∶1）的混和溶液超声提取,提取液用弗罗里硅土柱净化,用电子捕获检测器（ECD）检测。3个水平添加的回收率（n=5）分别为98.60%～110.2%、95.8～107.5和96.40～102.5%,RSD分别为3.0%～7.5%、3.2%～7.4%和3.1%～7.0%,方法的检出限为：0.000 4～0.004 0μg·mL^-1,线性相关系数R2为0.996 3～0.999 7。该方法时间短,操作简单,满足农药残留分析的要求。

A method to determine residues of eight organochlorines in astragalus with gas chromatography was proposed. The sample was ultrasonically extracted with petroleum ether-ethyl acetate solution （V/V = 2/1 ）. Extract was purified with Florisil SPE column and tested with electron capture detector （ECD）. The recovery rates （n = 5 ） obtained from the samples at three concentration levels were 98.60 % - 110.2 % , 95.8 % - 107.5 % and 96.40 % -102.5 % , with relative standard deviations （RSD） of 3.0 % -7.5 % , 3.2 % -7.4 % and 3.1% - 7.0 % , respectively. The detection limits for organochlorines were 0.000 4 - 0. 004 μg·mL^-1, with the correlation coefficients （ R^2） ranged form 0.9 963 to 0.9 997. Efficiently, this method can meet the requirements for pesticide residue determination.