牛奶中劳拉西泮的高效液相色谱分析  

High performance liquid chromatography analysis of lorazepam in milk

作　　者：郑佳妍 李昳晴 冯瑶 韩晓利 王庭欣[1] 刘峥颢[1] ZHENG Jiayan;LI Yiqing;FENG Yao;HAN Xiaoli;WANG Tingxin;LIU Zhenghao(College of Quality and Technical Supervision,Hebei University,Baoding 071002,China)

机构地区：[1]河北大学质量技术监督学院,河北保定071002

出　　处：《河北大学学报（自然科学版）》2024年第5期495-503,共9页Journal of Hebei University(Natural Science Edition)

基　　金：河北省重点研发计划项目(18275502D)。

摘　　要：为了建立检测牛奶中劳拉西泮的高效液相色谱分析方法,用体积分数0.2%甲酸-乙腈溶液离心提取样品中劳拉西泮残留(重复3次),C18固相萃取柱净化,洗脱液经氮气吹干后用体积分数50%甲醇水溶液溶解,0.22μm滤膜过滤,供高效液相色谱测定.采用安捷伦ZORBAX SB-C18色谱柱(4.6 mm×150 mm,5μm)为分析柱,V(甲醇)∶V(水)=68∶32为流动相,紫外检测器在230 nm波长处检测.结果表明:劳拉西泮在40~500μg/mL内线性关系良好,回归方程为y=4.047x-36.11,相关系数为0.999,检出限为0.927μg/mL,定量限为3.097μg/mL,牛奶中添加质量浓度分别为70、180、300μg/mL,添加回收率为81.27%~97.58%,相对标准偏差为1.1%,日内、日间相对标准偏差为1.2%~2.6%.该方法灵敏度高,准确度好,简便,快捷,适用于牛奶中劳拉西泮的检测分析.In order to establish detection of lorazepam in milk,high performance liquid chromatography(HPLC)method was used,The conditims are:dissolved in 0.2%formic acid,centrifugal extraction of lorazepam residual in acetonitrile solution,repeat 3 times,C18 solid phase extraction column,eluent after nitrogen blow dry with volume fraction of 50%methanol aqueous solution dissolve,0.22 mu m filter membrane filtration.An Agilent ZORBAX SB-C18 column(4.6 mm×150 mm,5μm)was used as the analytical column with methanol:water(V/V)=68∶32 as the mobile phase.The detection was carried out at 230 nm with a UV detector.The results showed that:the linear range of lorazepam was 40~500μg/mL,the regression equation was y=4.047 x-36.11,the correlation coefficient was 0.999,the limit of detection was 0.927μg/mL,the limit of quantification was 3.097μg/mL,and the additive levels in milk were 70,180,300μg/mL,respectively.The recoveries ranged from 81.27%to 97.58%with relative standard deviations(RSD)of 1.1%,intra-day and inter-day RSD of 1.2%to 2.6%.The method is sensitive,accurate,simple and quick,and suitable for the determination and analysis of lorazepam in milk.

关 键 词：劳拉西泮 牛奶 高效液相色谱法 外标法 

分 类 号：O627[理学—有机化学]