论文部分内容阅读
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 residues of organochlorine pesticides in the two-sided needles of traditional Chinese medicine for providing scientific basis for its quality control and standard formulation. Methods: The samples were extracted by acetone and purified by sodium sulfate anhydrous-PSA-C18-carbonized solid-phase extraction cartridges. GC-MS method was used to select the ion monitoring mode and external standard method. Eight kinds of organochlorine pesticide residues in the roots of Chinese herbs were tested. Results: One injection can simultaneously quantify and characterize the eight organochlorine pesticides in the two-sided needle. Among the 12 samples, 6 samples except 1, 4, 5, 6, 11 and 12 contained a small amount of OP’-DDT, and no other organochlorine pesticide residues were detected in other samples. The RSD of the instrument was between 0.89% and 2.21 %, The average recoveries of eight organochlorine pesticides ranged from 85.33% to 103.70% with RSD less than 4%. CONCLUSION: The content of organochlorine pesticide residues in Zanthoxylum nitidum in Guangxi is less than 0.2 ppm. GC-MS method can achieve the purpose of simultaneous quantitative and qualitative determination. The method has high sensitivity and good purification effect and can be applied to the determination of trace organochlorine Pesticide residue testing.