衍生化气相色谱-质谱法检测血液中草铵膦  

Analysis of Blood-harbored Glufosinate Ammonium Derivatized into GC-MS Detection

作　　者：乔静[1] 张文芳[1] 张瑛 杨士云[1] 刘永涛 QIAO Jing;ZHANG Wenfang;ZHANG Ying;YANG Shiyun;LIU Yongtao(Criminal Investigation Department of Beijing Public Security Bureau&Key Laboratory(Ministry of Public Security)of Forensic Toxicology,Beijing 100192,China)

机构地区：[1]北京市公安局刑事侦查总队,法庭毒物分析公安部重点实验室,北京100192

出　　处：《刑事技术》2021年第4期378-382,共5页Forensic Science and Technology

摘　　要：目的建立血液中草铵膦的衍生化气相色谱-质谱(GC-MS)检测方法。方法在空白血液中添加标准草铵膦,甲醇/乙腈(2∶8,体积比)提取,提取液挥干后甲醇复溶,加入等量乙酸酐在80℃干燥箱中衍生化1h,衍生产物于蒸发皿中80℃水浴挥干,用0.2mL乙腈定容后GC-MS分析。结果该方法血液中草铵膦乙酸酐衍生化的最小检出限为0.2μg/mL(S/N=45∶1),在0.5~10μg/mL范围内线性良好,外标法工作曲线为y=324826x+30384,R^(2)=0.9975,RSD%(n=3)为3.2%。结论该方法简便、可靠、易普及,适用于刑事案件中草铵膦的检验。Objective To establish a method for detecting blood-harbored glufosinate ammonium through derivatization to undergo into GC/MS analysis.Methods Glufosinate ammonium was extracted from whole blood with methyl alcohol/acetonitrile(2/8,V/V),successively subjected to evaporation at water bath of 80℃,consecutively having its residues resolved into methyl alcohol with which the same amount of acetic anhydride was followed to add for derivatization to perform under the time and temperature respective of 1h and 80℃.Finally,the derivatized product was dried and then resolved with acetonitrile(0.2mL)for detection of GC/MS along with external standard.Results With derivatization of acetic anhydride,the tested glufosinate ammonium got its correlation coefficient about 0.993 from the linear curve within concentrations ranging among 0.5~10μg/mL,having the relative standard deviation of 3.2%(n=3)and limit of qualification of 0.2μg/mL(S/N=45/1).Conclusion The method is simple and reliable for qualitative and quantitative analysis of glufosinate ammonium in whole blood.

关 键 词：法医毒物学 草铵膦 乙酸酐 衍生化 气相色谱-质谱 

分 类 号：DF795.1[医药卫生—法医学]