QuEChERS联合GC-MS/MS法测定心可宁胶囊中的17种有机氯农药残留量  

Determination of 17 organochlorine pesticide residues in Xinkening capsules by QuEChERS combined with GC-MS/MS

作　　者：马杰 罗疆南 李瑞莲 王湘波 MA Jie;LUO Jiang-nan;LI Rui-lian;WANG Xiang-bo(Hunan Institute of Drug Control,Changsha 410001;Hunan Pharmaceutical Quality Evaluation Engineering Technology Center,Changsha 410001)

机构地区：[1]湖南省药品检验研究院,长沙410001 [2]湖南省药品质量评价工程技术中心,长沙410001

出　　处：《中南药学》2020年第7期1156-1160,共5页Central South Pharmacy

基　　金：国家药品监督管理局2017年度国家药品抽验任务(编号:3)。

摘　　要：目的建立QuEChERS法联合GC-MS/MS测定心可宁胶囊中17种有机氯农药残留。方法样品经乙腈涡旋提取、QuEChERS净化、正己烷定容后,采用GC-MS/MS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 17种有机氯农药均在5~500 μg·L^(-1)与测定值呈良好的线性关系,相关系数均大于0.99;加样回收率为70.43%~96.08%,RSD(n=3)在0.91%~11%;重复性RSD值在1.8%~11.7%;检测限均不高于0.005 mg·kg^(-1),定量限均不高于0.01 mg·kg^(-1);进样精密度RSD<3%。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,适用于心可宁胶囊中17种有机氯农药残留的检测。Objective To establish a method to determine 17 organochlorine pesticide residues in Xinkening capsules by QuEChERS and GC-MS/MS.Methods The samples were extracted by acetonitrile vortex,purified by QuEChERS and volume fixed by n-hexane,before being determined by gas chromatography tandem mass spectrometry under ion detection.The retention time and characteristic ions were used for the qualitative identification of the target components,and the external standard method was used for quantitative analysis.Results The 17 organochlorine pesticides showed a good linearity at 50-500μg·L-1,and the correlation coefficient was more than 0.99.The recovery was 70.43%-96.08%,RSD(n=3)was 0.91%-11%,and the repeatability RSD was 1.8%-11.7%.The detection limit was less than 0.005 mg·kg-1 and the quantitative limit was less than 0.01 mg·kg-1.The injection precision RSD was less than 3%.Conclusion The sensitivity,accuracy and precision of this method all meet the technical requirements of pesticide multi-residue detection,which is suitable for the detection of 17 organochlorine pesticide residues in Xinkening capsules.

关 键 词：心可宁胶囊 农药残留量 QUECHERS GC-MS/MS 

分 类 号：R927[医药卫生—药学]