QuEChERS法联合在线GPC-GC-MS检测冠心丹参胶囊中20种有机氯农药残留  

Determination of 20 organochlorine pesticide residues in Guanxin Danshen pill by online GPC-GC-MS with offline disperse solid phase extraction

作　　者：肖丽和[1,2] 刁璇[1,2] 谢耀轩[1,2] 林亚珠[1,2] 王淑红[1,2] 王铁杰[1,2] 

机构地区：[1]深圳市药品检验所,深圳518057 [2]深圳药品质量标准研究重点实验室,深圳518057

出　　处：《中国新药杂志》2014年第15期1749-1753,1800,共6页Chinese Journal of New Drugs

基　　金：国家"重大新药创制"科技重大专项(2014ZX09304-307-02)

摘　　要：目的：建立QuEChERS法联合在线GPC-GC-MS测定冠心丹参胶囊中20种有机氯农药残留的分析方法。方法：样品经乙腈涡旋提取，加入N-丙基乙二胺（PSA）、C18-N进行分散固相萃取净化后，经在线凝胶渗透色谱（GPC）净化，采用气相色谱与质谱串联技术在离子检测方式下测定，以保留时间和特征离子进行目标成分的定性鉴别，以外标法定量。结果：20种有机氯农药在2～100μg·L^-1范围内均呈良好的线性关系，相关系数为0．9997～0．9999；3个水平加标回收率为82．3％～113．1％，RSD（n=3）为0．5％～9．1％；检出限为0．04～0．78μg·kg^-1，定量限为0．13～10．4μg·kg^-1，进样精密度RSD〈5％。结论：本方法的灵敏度、准确度和精密度均符合农药多残留检测技术要求，适用于冠心丹参胶囊中20种有机氯农药残留的检测。Objective： To establish an analysis method based on online gel permeation chromatography gas chromatography mass spectrometer （GPC-GC-MS） with offline disperse solid phase extraction for the determination of 20 organochlorine pesticide residues in Guanxin Danshen pill. Methods ： The samples were extracted with aceto- nitrile by the vortex extraction, and the extract was further purified by dispersive solid phase extraction with sorbents of primary secondary amine （PSA） and C18. The samples were detected by GPC-GC-MS with a mass selective ion monitoring （SIM） mode. The target pesticides were identified by comparing retention time and characteristic ions with reference using an external standard quantitative method. Results： The 20 organochlorine pesticide residues at 2- 100 μg·L^-1 showed a good linear relationship, the correlation coefficient were between 0. 999 7 and 0. 999 9 ; 3 levels recoveries ranged from 82.3% - 113.1% , RSD% （ n = 3 ） were 0.5 % - 9. 1% . The limits of detection （LOD） were 0.04 - 0.78 μg·L^-1. The limits of quantification （LOQ） were 0.13 - 10.4 μg·L^-1. The sampling precision RSDs were less than 5%. Conclusion： The method is sensitive, accurate and precise for the requirement of multi-pesticide residue detection technology. It is suitable for detecting 20 organochlorine pesticide residues in Guanxin Danshen pill.

关 键 词：QUECHERS 在线GPC—GC-MS 冠心丹参胶囊 有机氯农药残留 

分 类 号：R917[医药卫生—药物分析学]