食品科学 ›› 2008, Vol. 29 ›› Issue (8): 510-512.

• 分析检测 • 上一篇    下一篇

高效液相色谱-电喷雾串联质谱测定尿液中硝西泮代谢物7-氨基硝西泮的研究

李秋生, 沈崇钰, 徐锦忠, 袁媛, 胥传来   

  1. 江南大学食品学院; 江苏出入境检验检疫局食品实验室
  • 出版日期:2008-08-15 发布日期:2011-08-26

Determination of 7-Aminonitrazepam,Metabolite of Nitrazepam in Human Urine by High Performance Electrospray Liquid Chromatography-Tandem Mass Spectrometry

LI  Qiu-Sheng, SHEN  Chong-Yu, XU  Jin-Zhong, YUAN  Yuan, XU  Chuan-Lai   

  1. 1.School of Food Science and Technology,Jiangnan University,Wuxi 214122,China;2.Food Laboratory,Jiangsu Entry-Exit Inspection and Quarantine Bureau,Nanjing 210001,China
  • Online:2008-08-15 Published:2011-08-26

摘要: 采用高效液相色谱-电喷雾串联质谱测定尿液中硝西泮的代谢物7-氨基硝西泮。测定时尿液中加入内标7-氨基氯硝西泮,经过β-葡萄糖醛酸酸苷酶水解,碱性液萃取,过0.45μm的滤膜,反相色谱分离后进行质谱分析,在选择反应监测模式(SRM)下进行特征母-子离子对信号采集。根据保留时间、母离子和特征子离子信息进行定性分析,内标法进行定量。药物检测限(LOD,S/N=3)为0.07μg/L,定量限(LOQ)为0.5μg/L,线性范围为1~50μg/L。在1.0、10.0、25.0、45.0μg/L四个添加水平下,回收率范围为89.0%~95.2%,相对标准偏差(RSD)小于6.4%。结果表明,该法简单、灵敏、重现性强,适用于尿液中7-氨基硝西泮的分析确证。

关键词: 高效液相色谱, 串联质谱, 硝西泮, 7-氨基硝西泮

Abstract: A method was developed for the determination of urinary 7-aminonitrazepam(7-ANZP),the major metabolite of nitrazepam,by high performance liquid chromatography-electrospray tandem mass spectrometry. After being added 7-aminoclonazepam(7-ACZP,internal standard),hydrolyzed with β-glucuronidase,liquid-liquid extracted at pH 10.8,and filtrated with 0. 45 μm membrane,the samples were analyzed. Mass spectral acquisition was performed with selective reaction monitoring of two diagnostic transition reactions. The qualitative analysis was based on the retention time,and the quantification was carried out with intension of the internal standard. The recoveries of 7-ANZP in spiked blank samples at different concentration levels are in the range of 89.0%~95.2% with relative standard deviations(RSD) no more than 6.4%. The limit of detection in urine(LOD) is 0.07 μg/L,and the limit of quantification(LOQ) is 0.5μg/L. The linear range is from 1μg/L to 50μg/L. This method is suitable for analysis of 7-ANZP with characteristics of easy operating,high sensitivity and repeatability.

Key words: high performance liquid chromatography, electrospray tandem mass spectrometry, nitrazepam, 7-aminonitrazepam