生物样品测定分析方法中提取回收率的探讨_杨培.docVIP

生物样品测定分析方法中提取回收率的探讨_杨培 ? 722 ?中华中医药杂志(原中国医药学报)2015年3月第30卷第3期 CJTCMP,March 2015,Vol.30,No.3 ?论著? 生物样品测定分析方法中提取回收率的探讨 杨培1，林龙飞1，田宇2，张慧1，王卫华2，倪健1 （1北京中医药大学中药学院，北京 100102；2清华大学生物医学测试中心，北京 100084） 摘要：目的：验证提取回收率的范围限定是否应当列入生物样品测定方法学规范中。方法：以芍药苷为代表药物，大鼠血浆为基质，分别采用蛋白沉淀法（PP）和固相萃取法（SPE）进行生物样品的前处理，对所得的精密度、准确度和提取回收率3个主要指标进行数据分析，并进行口服给药后大鼠体内芍药苷药时曲线的测定。结果：不同前处理方法所得的样品，在精密度、准确度两项指标上并无数理统计差异，提取回收率存在显著差异，但对大鼠口服芍药苷的药动学指标检测并无影响，两种方法均测得芍药苷均在30min有最大吸收，Cmax-PP=（597.49±58.90）ng/mL，Cmax-SPE=（615.50±22.52）ng/mL。结论：在药物研发中，根据被测药物的浓度、基质效应的影响，合理选择前处理方法，而不将提取回收率限定范围作为方法学确证的判断指标是值得提倡的环保经济的研究原则。 关键词： 药代动力学；回收率；蛋白沉淀法；固相萃取法；液质联用技术 基金资助：国家科技重大专项课题（No.2012Z026） Discussion of recovery in biological sample determination methodology YANG Pei1, LIN Long-fei1, TIAN Yu2, ZHANG Hui1, WANG Wei-hua2, NI Jian1 ( 1School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 100102, China; 2Center of Biomedical Analysis, Tsinghua University, Beijing 100084, China ) Abstract: Objective: To verify whether it is necessary to define a specific range of recovery in biological sample determination methodology. Methods: Paeonifl orin was adopted as a pharmic sample along with the employment of rats’ plasma as matrix in this study. The selection of precipitation protein (PP) and solid-phase extraction (SPE) as designate method to process the determination of paeonifl orin. After that, the data generated by precision, accuracy and rate of recovery were processed by data analysis. Results: The results indicate that there was no diff erence on the index of precision and accuracy according to mathematical statistics. Therefore, there was no impact to study in vivo pharmacokinetics although a signifi cant diff erence was shown on the rate of recovery. The maximum effi cacy of two methods was 30in and Cmax-PP=(597.49±58.90)ng/mL, Cmax-SPE=(615.50±22.52) ng/mL. Conclusion: It is encouraged to conduct the future development of drugs by choosing fe