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,0.22 μm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.

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,5 μm)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 40~500 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 sensitive, accurate, simple and quick, and suitable for the determination and analysis of lorazepam in milk.- DOI:10.3969/j.issn.1000-1565.2024.05.006牛奶中劳拉西泮的高效液相色谱分析郑佳妍,李昳晴,冯瑶,韩晓利,王庭欣,刘峥颢(河北大学 质量技术监督学院,河北 保定 071002)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,0.22 μm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.关键词:劳拉西泮;牛奶;高效液相色谱法;外标法中图分类号:O627 文献标志码:A 文章编号:1000-1565(2024)05-0495-09High performance liquid chromatography analysis of lorazepam in milk ZHENG Jiayan, LI Yiqing, FENG Yao, HAN Xiaoli, WANG Tingxin, LIU Zhenghao(College of Quality and Technical Supervision, Hebei University, Baoding 071002, China)Abstract: 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,5 μm)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 40~500 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 sensitive, accurate, simple and quick, and suitable for the determination and analysis of lorazepam in milk.- 收稿日期:2024-06-05;修回日期:2024-06-25 基金项目:河北省重点研发计划项目(18275502D) 第一作者:郑佳妍(1997—),女,河北大学在读硕士研究生,主要从事食品安全快速检测技术研究. E-mail:574166857@qq.com 通信作者:王庭欣(1965—),女,河北大学教授,主要从事食品安全快速检测技术研究.E-mail:tingxingwang@126.com刘峥颢(1973—),女,河北大学副教授,主要从事食品安全及标准化研究.E-mail:sgl1997@126.com 第5期郑佳妍等:牛奶中劳拉西泮的高效液相色谱分析河北大学学报(自然科学版) 第44卷