近红外分析用于中药产品质量实时放行测试的可靠性研究.docVIP

近红外分析用于中药产品质量实时放行 测试的可靠性研究 孙飞 徐冰 戴胜云 史新元 乔延江 北京中医药大学中药信息工程中心中药生产过程与 质量控制北京市重点实验室 摘要： 目的:研究近红外定量分析误差和中药产品质量控制限度之间的关系，建立可靠 的中药质量实时放行测试(RTRT)方法。方法：以三七总皂昔(PNS)速释片为载 体，采用偏最小二乘法(PLS)建立近红外(WR)漫反射光谱预测三七总皂昔 含量的定量模型;通过实验设计计算不同浓度NIR定量分析误差，基于B-期望 容忍区间估计质量控制上下限处的定量分析风险，在一定置信水平下建立有效 组分含量实时放行控制限。结果:所建N1R定量模型性能偏差比(RPD)为4. 34, 说明预测性能良好;在90%置信水平下，NIR分析的样品RTRT下限为0. 2665g/g, 上限为0. 2918g/g,较标准质控限度有所缩减。结论:本研究所建中药片剂含量 实时放行测试方法，可提高放行可靠性和效率，并可推广用于其他产品放行检 验。 关键词： 近红外光谱法;实吋放行测试;可靠性;三七总皂昔速释片;分析质量源于设 计； 作者简介：徐冰，北京市朝阳区北三环东路11号北京屮医药大学屮药信息工程 中心，邮编:100029;电话:010-mail:btcm@163. com 作者简介：乔延江;北京市朝阳区北三环东路11号北京中［矢药大学中药信息工程 中心，邮编:100029,电话:010-mail :yjqiao@263. net 收稿日期：2016年11月28日 基金：国家自然科学基金项冃(No. Reliability study of real time release testing for Chinese medicine preparation based on near infrared spectroscopy SUN Fei XU Bing DAI Sheng-yun SHI Xin—yuan QIAO Yan-jiang Research Center of Traditional Chinese Medicine Informstion Engineering, Beijing university of Chinese Medicine; Abstract： Objective: To study the relationship between the quantitative analysis errors of near infrared reflectance (NIR) and the limit of quality control of TCM, and to establish a robust and reliable real-time release test (RTRT) method on TCM product qual i ty. Methods: Taking Panax notoginseng saponins (PNS) immediate releeise tablet as the object, the partial least squares (PLS) model was adopted to predict the content of Panax notoginseng saponins with the NIR spectroscopy.The systematic errors and accidentdl errors of NIR quantitative analysis at different concentration levels were an alyzed by experimental design. A dec is i on paragraph was developed, combining two types of errors and 3 -expectation tolerance interveil to estimate the risk at the upper and lower limit of the quality control of tablets. Results: The relative prediction deviation of the proposed model was 4.34, which indicated that the predictive ability of model was good. The qual i ty conirol limit of RTRT based on NIR me