UPLC-MS/MS法测定比格犬血浆中6-巯基嘌呤含量不确定度评定

doi:10.19803/j.1672-8629.20230593

中国药物警戒 ›› 2023, Vol. 20 ›› Issue (12): 1321-1325.
DOI: 10.19803/j.1672-8629.20230593

• 临床药物质量监测及评价专栏 • 上一篇下一篇

UPLC-MS/MS法测定比格犬血浆中6-巯基嘌呤含量不确定度评定

王佳庆¹, 汪祺^2△, 史卫忠³, 张冬婕³, 宁霄^4,*

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:2023-09-21 出版日期:2023-12-15 发布日期:2023-12-15
通讯作者: ^*宁霄,女,硕士,副主任药师,分析化学。E-mail: nx200730079@163.com
作者简介:王佳庆,女,硕士,副主任药师,临床试验及药物分析。^△为并列第一作者。
基金资助:
国家重点研发计划（2021YFC2401100）

Uncertainty evaluation for the determination of 6-MP in Beagle dog plasma by UPLC-MS/MS

WANG Jiaqing¹, WANG Qi^2△, SHI Weizhong³, ZHANG Dongjie³, NING Xiao^4,*

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;
⁴The Institute for Food and Cosmetics Testing, National Institute of Food and Drug Control, Beijing 100050, China

Received:2023-09-21 Online:2023-12-15 Published:2023-12-15

摘要/Abstract

摘要： 目的评定用超高效液相质谱联用（UPLC-MS/MS）法测定比格犬中血浆6-巯基嘌呤（6-MP）的不确定度。方法分析用UPLC-MS/MS测定比格犬血浆6-MP浓度中不确定度的来源并进行合成。结果比格犬血浆中6-MP低浓度（15 ng·mL^-1）和高浓度（375 ng·mL^-1）的扩展不确定度分别为1.04 ng·mL^-1和30.14 ng·mL^-1（P = 95%,k = 2）。结论 UPLC-MS/MS法测定比格犬血浆中6-MP浓度的不确定度,在低浓度时主要由曲线拟合、回收率及基质效应引入,高浓度时主要来源于回收率、曲线拟合和生物样本配置。

关键词: 超高效液相质谱联用, 6-巯基嘌呤, 含量测定, 不确定度, 比格犬, 血浆

Abstract: Objective To evaluate the uncertainty for the determination of 6-mercaptopurine (6-MP) in beagle dog plasma by UPLC-MS/MS. Methods The whole process during the 6-MP determination was analyzed and the uncertainty from various sources were calculated. The combined and expanded uncertainty were also evaluated. Results The expanded uncertainty of 6-MP at low (15 ng·mL^-1 ) and high (375 ng·mL^-1) levels were 1.04 ng·mL^-1and 30.14 ng·mL^-1, respectively (P = 95%, k = 2). Conclusion The uncertainty for the determination of 6-MP in beagle dog plasma by UPLC-MS/MS at low concentration is mainly caused by calibration curve fitting, recovery and matrix effect, while at high concentration the uncertainty is mainly caused by recovery, calibration curve fitting and sample preparation.

Key words: UPLC-MS/MS, 6-MP, determination, uncertainty, Beagle dog, plasma

中图分类号:

R927.1

王佳庆, 汪祺, 史卫忠, 张冬婕, 宁霄. UPLC-MS/MS法测定比格犬血浆中6-巯基嘌呤含量不确定度评定[J]. 中国药物警戒, 2023, 20(12): 1321-1325.

WANG Jiaqing, WANG Qi, SHI Weizhong, ZHANG Dongjie, NING Xiao. Uncertainty evaluation for the determination of 6-MP in Beagle dog plasma by UPLC-MS/MS[J]. Chinese Journal of Pharmacovigilance, 2023, 20(12): 1321-1325.

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PLC-MS/MS法测定比格犬血浆中6-巯基嘌呤含量不确定度评定UPLC-MS/MS法测定比格犬血浆中6-巯基嘌呤含量不确定度评定

UPLC-MS/MS法测定比格犬血浆中6-巯基嘌呤含量不确定度评定

Uncertainty evaluation for the determination of 6-MP in Beagle dog plasma by UPLC-MS/MS

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