中国药物警戒 ›› 2023, Vol. 20 ›› Issue (12): 1346-1350.
DOI: 10.19803/j.1672-8629.20230541

• 临床药物质量监测及评价专栏 • 上一篇    下一篇

UPLC-MS/MS法测定人脑脊液中去甲万古霉素含量不确定度评价

王佳庆1, 汪祺2△, 张冬婕3, 梅升辉3*, 宁霄4#   

  1. 1首都医科大学附属北京天坛医院临床试验中心，北京 100050;
    2中国食品药品检定研究院中药民族药检定所 北京 100050;
    3首都医科大学附属北京天坛医院药学部，北京 100050;
    4中国食品药品检定研究院食品化妆品检定所，北京 100050
  • 收稿日期:2023-09-01 出版日期:2023-12-15 发布日期:2023-12-15
  • 通讯作者: *梅升辉,男,博士,主任药师,药物化学与药物分析。E-mail: meishenghui1983@126.com; #为共同通信作者。
  • 作者简介:王佳庆,女,硕士,副主任药师,临床试验与药物分析研究。△为并列第一作者。
  • 基金资助:
    国家重点研发计划（2021YFC2401103）

Uncertainty evaluation on the determination of norvancomycin in human cerebrospinal fluid by UPLC-MS/MS

WANG Jiaqing1, WANG Qi2△, ZHANG Dongjie3, MEI Shenghui3,*, NING Xiao2#   

  1. 1Clinical Trial Center, Beijing Tiantan Hospital, Capital Medical University, Beijing 100050, China;
    2Institute for control of Chinese traditional medicine and ethnic medicine, National Institutes for Food and Drug Control, Beijing 100050, China;
    3Department of Pharmacy, Beijing Tiantan Hospital, Capital Medical University, Beijing 100050, China;
    4Institute for Food and Cosmetics Testing, National Institutes for Food and Drug Control, Beijing 100050, China
  • Received:2023-09-01 Online:2023-12-15 Published:2023-12-15

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摘要： 目的 评定UPLC-MS/MS测定人脑脊液中去甲万古霉素（NVCM）含量的不确定度。方法 分析UPLC-MS/MS法测定人脑脊液中去甲万古霉素含量的不确定度来源,计算不确定度并进行合成和扩展。结果 去甲万古霉素在低浓度（3 mg·L-1）和高浓度（300 mg·L-1）的扩展不确定度分别为1.18、70.97 mg·L-1（P = 95%,k = 2）。结论 UPLC-MS/MS法测定人脑脊液中去甲万古霉素含量的不确定度在低含量时主要由曲线拟合、重复性和回收率引入。在高含量时主要由重复性,回收率和基质效应引入。本研究建立的脑脊液中去甲万古霉素含量测定方法,为该药物使用的安全性和有效性提供了有效的监管手段。

关键词: 去甲万古霉素, 脑脊液, 超高效液相质谱色谱法, 不确定度评定, 含量, 安全性

Abstract: Objective To evaluate the uncertainty in norvancomycin (NVCM) determination in human cerebrospinal by UPLC-MS/MS. Methods The whole process during the NVCM determination was analyzed and the uncertainty sources were established, then the combined and expanded uncertainty were also evaluated. Results The expanded uncertainty with low (3 mg·L-1) and high (300 mg·L-1) levels of NVCM (P=95%, k=2) were 1.18 mg·L-1 and 70.97 mg·L-1, respectively. Conclusion The uncertainty in NVCM determination in human cerebrospinal by UPLC-MS/MS was mainly caused by curve fitting, repeatability and recovery for low concentrations and repeatability, matrix effect and recovery for high concentrations. The method for determining the content of NVCM in cerebrospinal fluid established by our research institute provides an effective regulatory means for the safety and effectiveness of the drug’s use.

Key words: NVCM, human cerebrospinal fluid, UPLC-MS/MS, UNcertainty evaluation, content, safety

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