水浸GC-MS法检测生物检材中的百草枯  

Determination of Paraquat in Biomaterial by GC-MS with Water

作　　者：解润芳 佟钧 诸晨 徐天勇 解继明 XIE Run- fang;TONG Jun;ZHU Chen;XU Tian-yong;XIE Ji-ming(School of Forensic Medicine,Kunming Medical University,Kunming Yunnan 650500;Dept. of Physical Eduction,Kunming Yunnan 650500;Experiment Center for Medical Science Research of Kunming Medical University,Kunming Yunnan 650500;Dept. of Cardiothoracic Surgery,The 3rd People’s Hospital of Yunnan Province,Kunming Yunnan 650011,China)

机构地区：[1]昆明医科大学法医学院,云南昆明650500 [2]昆明医科大学体育部,云南昆明650500 [3]昆明医科大学科研实验中心,云南昆明650500 [4]云南省第三人民医院心胸外科,云南昆明650011

出　　处：《昆明医科大学学报》2017年第7期27-32,共6页Journal of Kunming Medical University

基　　金：云南省科技厅-昆明医科大学应用基础研究联合专项基金资助项目(2014FB013,2016FZ007)

摘　　要：目的建立一种简便、快速、准确、可靠的水浸气相色谱-质谱联用法(GC-MS)检测生物检材中的百草枯.方法根据百草枯的水溶性,用水浸法对生物检材进行样品前处理,用GC-MS对样品进行分离分析,用总离子流图(TIC图)中百草枯的保留时间及质谱图中百草枯的特征离子碎片定性.结果该方法样品前处理简单,使用的有机溶剂少,背景干扰小,分离效果好,分析速度快,百草枯定性的保留时间为6.674 min,百草枯的特征离子碎片为156(m/z=156);方法回收率为91.42%,日内及日间相对标准偏差RSD分别为4.83%及6.87%,最低检出限(LLOD)为0.005 mg/m L.结论该方法简便、准确、可靠,可用于法医毒物分析生物检材中百草枯的检验.Objective To establish a simple,rapid,accurate and reliable method of gas chromatography-mass spectrometry(GC-MS)with water extraction in order to determine the paraquat in biomaterial.Method The biomaterial was firstly pre-treated by using water as reagent to extract paraquat,and then GC-MS was employed to determine these samples.The retention time of the paraquat in total ion current(TIC)and the characteristic fragment ions of paraquat in mass spectrogram were taken as qualitative basis.Result The method demonstrated several advantages:simple sample pre-treatment,little consumption of organic reagents,less background interference,good separation effect,and fast analytical speed.The retention time was6.674mins and the characteristic fragment ions was156(m/z=156).The recovery rate was91.42%and the relative standard deviation(RSD)of the intra-day and the inter-day were4.83%and6.87%respectively.The lowest limit of detection(LLOD)was0.005mg/mL.Conclusion The method can be applied to determine the paraquat in biomaterial of forensic toxicological analysis.

关 键 词：法医毒物分析 水浸法 GC-MS 生物检材 百草枯 

分 类 号：R991[医药卫生—毒理学]