GC-MS测定两面针中8种有机氯农药残留量  

Determination of Organochlorine Pesticide Residues in the Roots of Zanthoxylum nitidum by GC-MS

作　　者：焦爱军[1] 冯洁[1] 赖茂祥[2] 

机构地区：[1]广西医科大学药学院,广西南宁530021 [2]广西中医药研究院,广西南宁530022

出　　处：《中药材》2013年第4期528-531,共4页Journal of Chinese Medicinal Materials

基　　金：广西自然科学基金(2010GXNSFA013187);广西中医药管理局中医药科技专项(GZKZ1141)

摘　　要：目的:测定中药两面针中有机氯类农药残留,为其质量控制和标准的制定提供科学依据。方法:样品经丙酮超声提取,经无水硫酸钠-无水硫酸镁-PSA-C18-石墨化碳填料固相萃取小柱净化,应用GC-MS法、选择离子监测模式和外标法定量,对中药两面针根中8种有机氯农药残留进行检测。结果:一次进样可同时对两面针中8种有机氯农药准确定量和定性。12份样品中,除1、4、5、6、11、12共6批次样品含有少量的OP'-DDT外,其余样品均无其他有机氯农药残留;仪器精密度RSD在0.89%～2.21%之间,8种有机氯农药平均回收率在85.33%～103.70%之间,RSD均小于4%。结论:广西产两面针药材的有机氯农药残留含量均小于0.2 ppm,GC-MS法可达到同时定量和定性的目的,测定方法灵敏度高,净化效果好,可应用于两面针药材中有机氯微量农药残留的检测。Objective：To determine the contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum and provide scientific foundation for the quality control and standard establishment. Methods： GC-MS method with selected ion monitoring （SIM） mode was used to analyze the contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidurn. The samples were extracted with acetone and ultrasonic vibrations, and the analytical samples were purified by anhydrous sodium sulfate-anhydrous magnesium sulfate -PSA -C18-PestiCarb -phase extraction （SPE） cartridge. Results： Eight kinds of organochlorine pesticide were detected simuhanously. Small amounts of OP-DDT were detected in samples 1,4,5,6,11 and 12, no organochlorine pesticide residue was detected in other samples. The RSD of precision ranged from O. 89% to 2. 21% , and the average recovery ranged from 85.33% to 103. 70% ,with the RSD less than 4%. Conclusion：The contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum are less than 0. 2 ppm. This method is sensitive, good purifying, and suitable for analyzing organochlorine pesticide residues in the roots of Zanthoxylum nitidum.

关 键 词：两面针 气相色谱-质谱联用 有机氯农药 

分 类 号：R282.6[医药卫生—中药学]