超高效液相色谱-串联质谱法同时测定河虾中地西泮和奥沙西泮残留量  

Simultaneous determination of diazepam and oxazepam residues in river shrimp by ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：江恩源[1] 朱国强[1] 韦丽丽[1] 喻梁洪 JIANG Enyuan;ZHU Guoqiang;WEI Lii;YU Lianghong(Wuzhou Municipal Center for Disease Control and Prevention,Wuzhou 543002,China)

机构地区：[1]梧州市疾病预防控制中心,广西梧州543002

出　　处：《化学分析计量》2024年第11期107-112,共6页Chemical Analysis And Meterage

摘　　要：建立了超高效液相色谱-串联质谱同时测定河虾中地西泮和奥沙西泮残留量的方法。样品经乙腈提取,全自动MCX小柱净化,采用Shim-packGISSC18色谱柱(50mm×2.1mm,1.9μm)分离,以甲醇-0.1%(体积分数)甲酸溶液为流动相进行梯度洗脱,在电喷雾离子源正离子模式、多反应监测模式下进行扫描检测,内标法定量。地西泮和奥沙西泮的质量分数在0.1~10.0μg/kg范围内与色谱峰面积线性关系良好,相关系数均不小于0.9993,方法检出限均为0.05μg/kg。样品的加标平均回收率为83.1%~94.0%,测定结果的相对标准偏差为2.3%~7.8%(n=6)。该方法灵敏度高、准确度好,适用于河虾中地西泮和奥沙西泮残留量的测定。A method for simultaneous determination of diazepam and oxazepam residues in river shrimp by ultra high performance liquid chromatography-tandem mass spectrometry was established.The samples were extracted by acetonitrile,purified by automatic MCX column,separated by Shim-pack GISSC18 column(50 mm×2.1 mm,1.9μm),then gradient elution was performed with methanol-0.1%(volume fraction)formic acid solution as mobile phase,and scanning detection was performed in electrospray ion source positive ion mode and multi reaction monitoring mode.Quantitative by internal standard method.The mass fractions of diazepam and oxazepam in the range of 0.1-10.0μg/kg had a good linear relationship with the chromatographic peak area,and the correlation coefficients were all no less than 0.9993.The detection limits of the method were 0.05μg/kg.The average recoveries were 83.1%-94.0%,and the relative standard deviations were 2.3%-7.8%(n=6).The method has high sensitivity and accuracy,which is suitable for the determination of diazepam and oxazepam residues in river shrimp.

关 键 词：超高效液相色谱-串联质谱法 同位素内标 地西泮 奥沙西泮 全自动固相萃取 

分 类 号：O657.7[理学—分析化学]