陶青;金正吉;罗晓健;饶小勇;何雁;
TAO Qing;JIN Zheng-ji;LUO Xiao-jian;RAO Xiao-yong;HE Yan;Jiangxi University of Traditional Chinese Medicine;the National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine;

• 1:江西中医药大学
• 2:中药固体制剂制造技术国家工程研究中心

摘要(Abstract)：

利用近红外光谱技术对片剂包衣终点判别与包衣过程分析。首先,采用分层k折交叉验证,讨论光谱区间与预处理方法的优选组合,作为建模条件;其次,根据建模条件,分别建立该研究提出的基于主成分分析与置信区间的定性模型与一致性检验模型,并对包衣合格性判别性能进行计算;随后,由内部交叉验证得到包衣终点上合格率,用作包衣终点判别阈值;最后,利用上述模型计算测试集各个批次的模型参数及预测合格率,用于包衣终点的判别和过程分析。与一致性检验相比,该研究方法对包衣合格性的判别更准确、更稳定,且当以95%的合格率作为包衣终点的判别阈值时可准确判别包衣终点。在过程分析中,该研究方法与一致性检验的过程参数(模型判别参数、预测合格率)的变化趋势基本一致。结果表明,该研究方法性能良好、稳定,可用于包衣终点的判别与过程分析,对减少批间差异,提高产品一致性具有重要意义。与此同时,该研究方法也为未来进行在线的近红外检测的研究奠定了基础。
To conduct endpoint determination of tablet coating and analyze coating process by near-infrared spectroscopy(NIRS). Firstly, the layered k-fold cross validation was used to discuss the optimal combination of spectral interval and preprocessing method, and the optimal result was used as the modeling condition. Secondly, in above condition, the qualitative model was proposed based on the throught of principal component analysis(PCA) and confidence interval, this model and the conformity test model were established respectively in this study, and the discrimination performance of coating eligibility was calculated. Then, the internal cross validation was used to obtain the coating end-point conforming rate as the threshold for determining the endpoint of tablet coating. Finally, the results of predicted conforming rate and discrimination parameters for the test samples of different batches were calculated with the above models, which were then further used for end-point detection and process analysis. As compared with the conformity test, this method proposed in this study was more accurate and stable in determining the coating conformity, and the coating endpoint can be accurately determined when 95% of the eligibility rate was used as the discriminant threshold. Meanwhile, in the process analysis, the change trend of the process parameters(model discrimination parameters, prediction conforming rate) was basically consistent with that in the conformity test. The results indicate that the method proposed in this study has a good and stable performance, which can be used to determine the endpoint of coating and analyze the process. It is of great significance to reduce the difference between batches and improve the product consistency. Meanwhile, this research method also lays a foundation for the future researches by online near infrared measurements.

关键词(KeyWords)： 近红外光谱;包衣终点;过程分析;主成分分析;置信区间
near infrared spectroscopy;endpoint determine of coating;process analysis of coating;principal component analysis;confidence interval

Abstract:

Keywords:

基金项目(Foundation): 国家自然科学基金项目(81960715);; 国家“重大新药创制”科技重大专项(2018ZX09201010)

作者(Author): 陶青;金正吉;罗晓健;饶小勇;何雁;
TAO Qing;JIN Zheng-ji;LUO Xiao-jian;RAO Xiao-yong;HE Yan;Jiangxi University of Traditional Chinese Medicine;the National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine;

Email:

DOI: 10.19540/j.cnki.cjcmm.20200810.301

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