敌草快的异构体推断和检测稳定性研究  

Study on the differentiation and detection of diquat isomers and their stability during detection

作　　者：宣宇[1] 钱秉信 潘卫刚 孙剑聪 傅得锋 Xuan Yu;Qian Bingxin;Pan Weigang;Sun Jiancong;Fu Defeng(The criminal imestigaion depurmern 0f public security bureau of Zhejiang prowice.Zhejieong Key Laboraiony of Forensic Science and Technologs.Hangzhon,Zhegjiang 310009,China;The pubic security bureau of Wenlirg City,Taizhou 317500 China;The public securiy brureru of Shnoxing City,Shooxing,Zhejiang 312000,China)

机构地区：[1]浙江省公安厅刑侦总队,浙江省刑事科学技术应用研究重点实验室,浙江杭州310009 [2]温岭市公安局,浙江台州317500 [3]绍兴市公安局,浙江绍兴312000

出　　处：《中国法医学杂志》2022年第4期336-339,共4页Chinese Journal of Forensic Medicine

摘　　要：目的推断敌草快的构象异构体的存在方式并建立稳定的提取检验方法方法通过不同试剂、pH值条件观察敌草快的液相色谱出峰情况,并通过沉淀蛋白方法考察体内样品的稳定性。结果敌草快在不同的存储介质中存在两种构象异构体间的转换,在中性和酸性水溶液中易呈现反式构象,在碱性水溶液和有机试剂中易呈现顺式构象;在体内样品中主要呈现反式异构体,20 d测试时间内均能检出,但存在方式不稳定。结论敌草快经LC/MS检测时受存储试剂及pH的影响较大,两种构象异构体的色谱响应差别较大,在检测样品时可以在进样溶液中加入一定比例的挥发性酸,以提高敌草快的检测灵敏度并稳定保留时间,实现对敌草快样品的准确定性定量分析。Objective To investigate the existence of diquat isomers and establish a stable extraction method.Methods The chromatographic peaks of diquat were observed under different types of reagent and pH values.The stability of diquat from in-vivo samples was investigated by protein precipitation method.Results Diquat tended to converse between two conformational isomers when storage media changed,including trans conformation in neutral and acidic aqueous solution,and cis conformation in alkaline aqueous solution and organic reagent.In vivo samples,diquat mainly presented as trans isomers,which could be detected within 20 days with unstable conformation isomers.Conclusions The stability of diquat isomers was greatly affected by storage reagent and pH value when detected by LC/MS.The chromatographic behaviors of two conformation isomers of diquat are quite different.A certain proportion of volatile acid can be added into the injection solution to improve the sensitivity and stabilize the retention time of diquat,for accurate qualitative and quantitative determination.

关 键 词：敌草快 异构体 稳定性 液质联用仪 

分 类 号：DF795.2[医药卫生—法医学]