HPLC法测定中药材能力验证样品中红景天苷含量的不确定度评定  

Uncertainty Evaluation of Determination of Salidroside in Proficiency Testing Samples of Traditional Chinese Medicine by HPLC

作　　者：田树兴 丁艳谱 周崇富 刘红光 李军山 TIAN Shuxing;DING Yanpu;ZHOU Chongfu;LIU Hongguang;LI Junshan(Yunnan Shineway Spirin Pharmaceutical Co.Ltd.,Chuxiong 675000,China;Chuxiong Shineway Spirin Pharmaceutical Research Co.Ltd.,Chuxiong 675000,China;Shineway Pharmaceutical Group Ltd.,Shijiazhuang 051430,China)

机构地区：[1]云南神威施普瑞药业有限公司,楚雄675000 [2]楚雄神威施普瑞药物研究有限公司,楚雄675000 [3]神威药业集团有限公司,石家庄051430

出　　处：《计量科学与技术》2022年第3期23-29,共7页Metrology Science and Technology

基　　金：云南省重大科技专项(2019ZF008)。

摘　　要：为评定高效液相色谱(HPLC)法测定中药材能力验证样品中红景天苷含量的不确定度,采用《中华人民共和国药典》2015年版一部红景天含量测定方法,对红景天粉末能力验证样品进行测定,得出红景天苷含量。依据国家计量技术规范JJF 1059.1-2012《测量不确定度评定与表示》,对红景天粉末(样品No.153和No.275)2个样品中红景天苷含量测定的不确定度来源进行分析。通过建立数学模型量化不确定度分量,计算合成不确定度和扩展不确定度,并与能力验证结果进行对比。实验结果表明,样品No.153红景天粉末样品测定结果报告为1.41%±0.05%,k=2;样品No.275红景天粉末样品测定结果报告为2.58%±0.08%,k=2,且能力验证结果为满意;2个样品红景天苷含量测量不确定度均主要来源于重复性实验、标准曲线拟合以及对照品系列溶液稀释3部分。该研究可为评价红景天苷含量测定结果的质量和控制实验室内部质量提供参考;同时不确定度评定和能力验证结果表明,实验室在102.8μg/mL至1 028μg/mL的浓度水平上均有能力开展中药材中红景天苷的含量测定并能保证数据可靠。To evaluate the uncertainty of determination of Salidroside in proficiency testing samples of traditional Chinese medicine by high-performance liquid chromatography(HPLC), the content of salidroside was determined by the content determination method of Rhodiola in the first part of Pharmacopoeia of the People’s Republic of China(2015Edition). According to JJF 1059.1-2012 "Evaluation and Expression of Uncertainty in Measurement", the sources of uncertainty in the determination of Salidroside in two samples of Rhodiola powder No. 153 and No. 275 were analyzed. The mathematical model is established to quantify the uncertainty components, and the combined uncertainty and expanded uncertainty are calculated and compared with the results of capability verification. The result of No.153 Rhodiola powder sample was(1.41±0.05) % with k=2, the result of No.275 Rhodiola powder sample was(2.58±0.08)% with k=2, and the result of the proficiency test was satisfactory. The uncertainty of salidroside content in the two samples mainly came from repeatability tests, standard curve fitting, and dilution of reference series solution. This study can provide a reference for evaluating the quality of salidroside content determination results and controlling the internal quality of the laboratory. At the same time, uncertainty evaluation and proficiency testing results showed that the laboratory was capable of conducting the determination of salidroside in Chinese medicinal materials at the concentration level from 102.8 μg/mL to 1 028 μg/mL and ensure the reliability of data.

关 键 词：不确定度 红景天苷 高效液相色谱法 能力验证 

分 类 号：R284.1[医药卫生—中药学]