中药陈皮提取物粉末中糊精含量近红外分析方法的验证和不确定度评估  

Validation and uncertainty evaluation for the NIR quantitative analysis of dextrin in Chinese herbal tangerinepeel powder

作　　者：王馨[1] 徐冰[1,2] 薛忠[3] 杨婵[1] 张志强 史新元[1,2] 乔延江[1,2] 

机构地区：[1]北京中医药大学中药信息工程研究中心,北京100029 [2]中药生产过程控制与质量评价北京市重点实验室,北京100029 [3]河北医科大学药学院,石家庄050017 [4]北京康仁堂药业有限公司,北京101301

出　　处：《药物分析杂志》2017年第2期339-344,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金项目(81403112);北京市自然科学基金项目(7154217);中药生产过程控制与质量评价北京市重点实验室2015年度科技创新基地培育与发展专项项目(Z151100001615065)

摘　　要：目的:建立陈皮提取物粉末中辅料糊精含量近红外定量的方法验证和不确定度计算的全局评价策略。方法:通过采集已知不同含量糊精和陈皮混合样品的近红外光谱信息,建立偏最小二乘模型(PLS),基于β-容度容忍区间(β-CTI)建立准确度曲线对近红外(near infrared,NIR)分析方法进行验证,并通过β-CTI进行不确定度评估。结果:浓度水平为1%、3%、5%时,分析方法的准确度在可接受范围之外,该方法不可接受;浓度水平为7%和10%时,分析方法的准确度在可接受范围之内,该方法可以接受。所建NIR分析方法的最低定量限约等于5.73%。不确定度评估表明该方法在浓度较高时,方法的不确定度较好。结论:通过引入β-CTI同时进行方法验证和不确定度计算的全局评价策略可以有效保障方法的可靠性和准确性,有效降低分析方法在日常应用中的风险,为其他分析方法的评价提供借鉴。Objective：To establish an overall evaluation strategy for the validation and uncertainty evaluation of near infrared（NIR）quantification of dextrin in dried tangerine.Methods：Through collecting the NIR spectral information of mixed samples with different contents of dextrin in dried tangerine,the NIR quantitative PLS model was built.Based on the β-content tolerance interval（β-CTI）,the accuracy profile（AP）was established to validate the NIR analytical method and the uncertainty was also evaluated by the β-CTI.Results：When the dextrin content was 1%,3%,5% the accuracy was beyond acceptable limit and the method is unacceptable;When the dextrin content was 7%,10% the accuracy was within acceptable limit and the method is acceptable.The lower limit of quantification（LLOQ）of the method was approximately equal to 5.73%.Uncertainty evaluation showed that the method had a good uncertainty at higher contents.Conclusion：The overall evaluation strategy for validation and uncertainty assessment at the same time through the introduction of β-CTI can ensure the reliability and accuracy of method,reduce the risk of method in the daily use,and provide reference for the evaluation of other analytical methods.

关 键 词：近红外 方法验证 准确度曲线 不确定度 β-容度容忍区间 陈皮 

分 类 号：R917[医药卫生—药物分析学]