气相色谱法测定三七粉及含三七原粉类中成药中17种有机氯类农药残留

Determination of 17 organochlorine pesticide residues in Chinese patent medicine containing panax notoginseng original powder and panax notoginseng powder by GC

建立气相色谱测定含三七药材原粉的中成药及三七粉中有机氯类农药残留的方法。样品经水溶散,加入丙酮超声提取,提取液经二氯甲烷萃取,萃取液脱水,并减压浓缩,用正己烷置换溶剂,用硫酸纯化溶液,离心取上清液,用DM-1701对17种农药进行分离,流速为1.5 mL/min,进样口温度为230℃,进样方式为不分流进样,色谱柱温度为程序升温,初始温度60℃,保持0.5 min,以10℃/min的速率升至240℃,保持3 min,再以20℃/min的速率升至280℃,保持5 min,^(63)Ni-ECD电子捕获检测器温度为300℃。17种有机氯类农药均达到基线分离,其质量浓度在3.75~100.30 ng/mL范围内与色谱峰面积线性关系良好,线性相关系数为0.998~0.999 9,检出限为2.3~4.4 ng/mL,17种有机氯类农药平均回收率为90.3%~102.2%,相对标准偏差为1.8%~2.8%(n=6)。该方法简便,抗干扰,便于推广应用。

A method was established for the determination of organochlorine pesticide residues in Chinese patent medicine and Panax notoginseng powder.The sample was dissolved in water,and acetone was added for ultrasonic extraction.The extract was extracted with dichloromethane.The extract was dehydrated and concentrated under reduced pressure.The solvent was replaced with n-hexane,and the solution was purified with sulfuric acid.The supernatant was centrifuged to obtain the supernatant.DM-1701 was used to separate 17 pesticides at a flow rate of 1.5 mL/min.The injector temperature was 230℃,the injection method was splitless injection,the chromatographic column temperature was adjusted as the following programm:the initial temperature was 60℃,maintained for 0.5 min,increased to 240℃at a rate of 10℃/min,maintained for 3 min,and then increased to 280℃at a rate of 20℃/min,maintained for 5 min.~(63)Ni-ECD electron capture detector temperature was 300℃.17 organochlorine pesticides were baseline separated.The mass concentration had a good linear relationship with the chromatographic peak area in the range of 3.75-100.30 ng/mL with the corelation coefficient between 0.998 and 0.999 9.The detection limit of each component was in the range of 2.3-4.4 ng/mL.The average recovery rate of 17 organochlorine pesticides were from 90.3%to 102.2%,and the relative standard deviation were1.8%~2.8%(n=6).The method is simple,anti-interference,and easy to promote the application.