高效液相色谱-质谱法测定淡水鱼中地西泮  

Determination of diazepam in freshwater fish by high performance liquid chromatographymass spectrometry

作　　者：林涛[1] 蔡苇 王志飞 普家云 李金峰 陈兴连[1] 刘宏程[1] 刘振环[1] LIN Tao;CAI Wei;WANG Zhifei;PU Jiayun;LI Jinfeng;CHEN Xinglian;LIU Hongcheng;LIU Zhenhuan(Quality Standards and Testing Technology Research Institute,Yunnan Academy of Agricultural Sciences,Kunming 650205,China;Department of Pharmacology,Yunnan College of Business Management,Kunming 650000,China;Yunnan Fishery Research Institute,Kunming 650111,China;Shiping County Agricultural Product Quality and Safety Testing Station,Shiping 662200,China)

机构地区：[1]云南省农业科学院质量标准与检测技术研究所,昆明650205 [2]云南经济管理学院医学院,昆明650106 [3]云南省渔业科学研究院,昆明650111 [4]石屏县农产品质量安全检测站,云南石屏662200

出　　处：《化学分析计量》2024年第9期28-32,共5页Chemical Analysis And Meterage

基　　金：云南省庞国芳院士工作站(202305AF150015),云南省农业联合专项面上项目(202301BD070001-049)。

摘　　要：建立高效液相色谱-质谱法测定淡水鱼中地西泮。样品用乙腈提取,采用Florisil填料和氨基填料净化,当Florisil填料和氨基填料的质量比为2∶3时,能够有效地吸附淡水鱼基质中的脂肪、脂质和蛋白质等杂质,降低基质效应,提高质谱响应的信噪比。地西泮的质量浓度在0.05~20 ng/mL范围内与色谱峰面积线性关系良好,相关系数为0.9996,检出限为0.15μg/kg,定量限为0.5μg/kg。空白样品加标回收率为84.2%~95.5%,测定结果的相对标准偏差为5.25%~6.83%(n=6)。该方法快速准确,基质效应小,能够满足水产品中地西泮的测定要求。A method for the determination of diazepam in freshwater fish by high performance liquid chromatographymass spectrometry was established.The sample was extracted with acetonitrile and purified using Florisil and amino fillers.When the mass ratio of Florisil fillers to amino filler was 2∶3,impurities such as fats,lipids,and proteins in freshwater fish matrix could be effectively adsorbed,matrix effects coule be reduced,and the signal to noise ratio of mass spectrometry response was improved.The mass concentration of diazepam had a good linear relationship with the chromatographic peak area in the range of 0.05-20 ng/mL,with the correlation coefficient of 0.9996,the detection limit of 0.15μg/kg,and the quantification limit of 0.5μg/kg.The recoveries of blank sample spiked were 84.2%-95.5%,and the relative standard deviations of the measurement results were 5.25%-6.83%(n=6).This method is fast and accurate,with minimal matrix effects,and can meet the requirements for determining diazepam in aquatic products.

关 键 词：高效液相色谱-质谱法 淡水鱼 地西泮 基质效应 

分 类 号：O657.7[理学—分析化学]