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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作  者:王佳庆[1] 汪祺[2] 史卫忠[3] 张冬婕 宁霄[4] WANG Jiaqing;WANG Qi;SHI Weizhong;ZHANG Dongjie;NING Xiao(Clinical Trial Center,Beijing Tiantan Hospital,Capital Medical University,Beijing 100050,China;Institute for Control of Chinese Traditional Medicine and Ethnic Medicine,National Institutes for Food and Drug Control,Beijing 100050,China;Department of Pharmacy,Beijing Tiantan Hospital,Capital Medical University,Beijing 100050,China;The Institute for Food and Cosmetics Testing,National Institute of Food and Drug Control,Beijing 100050,China)

机构地区:[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

出  处:《中国药物警戒》2023年第12期1321-1325,共5页Chinese Journal of Pharmacovigilance

基  金:国家重点研发计划(2021YFC2401100)。

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。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^(-1)and 30.14 ng·mL^(-1),respectively(P=95%,k=2).Conclusion The uncertainty for the determination of 6-MP in beagle dog plasma by UPLCMS/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.

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 

分 类 号:R927.1[医药卫生—药学]

 

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