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

Reliability study of real time release testing for Chinese medicine preparation based on near infrared spectroscopy

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:以三七总皂苷(PNS)速释片为载体,采用偏最小二乘法(PLS)建立近红外(NIR)漫反射光谱预测三七总皂苷含量的定量模型;通过实验设计计算不同浓度NIR定量分析误差,基于β-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NIR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。

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 quality.Methods: Taking Panax notoginseng saponins(PNS) immediate release 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 accidental errors of NIR quantitative analysis at different concentration levels were analyzed by experimental design.A decision paragraph was developed,combining two types of errors and β-expectation tolerance interval 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 quality control limit of RTRT based on NIR method was from 0.2665 g/g to 0.2918 g/g,which was shrunken than the standard control limits.Conclusion: The real-time release testing of TCM tablet can improve the release efficiency and reliability,and it can also be extensive to other products release test.