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牛奶中劳拉西泮的高效液相色谱分析

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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,5 μm)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40~500 μg/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0.927 μg/mL,定量限为3.097 μg/mL,牛奶中添加质量浓度分别为70、180、300 μg/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.
High performance liquid chromatography analysis of lorazepam in milk
In order to establish detection of lorazepam in milk,high performance liquid chromatogra-phy(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 af-ter 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,5 μm)was used as the an-alytical 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 40~500 μg/mL,the regression equation was y=4.047x-36.11,the correlation coefficient was 0.999,the limit of detection was 0.927 μg/mL,the limit of quantification was 3.097 μg/mL,and the additive levels in milk were 70,180,300 μg/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 sensi-tive,accurate,simple and quick,and suitable for the determination and analysis of lorazepam in milk.

lorazepammilkhigh performance liquid chromatographyexternal standard method

郑佳妍、李映晴、冯瑶、韩晓利、王庭欣、刘峥颢

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河北大学质量技术监督学院,河北保定 071002

劳拉西泮 牛奶 高效液相色谱法 外标法

河北省重点研发计划项目

18275502D

2024

河北大学学报(自然科学版)
河北大学

河北大学学报(自然科学版)

CSTPCD北大核心
影响因子:0.322
ISSN:1000-1565
年,卷(期):2024.44(5)
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