Objective: In a chromatographic cycle, the adsorption process is a critical unit operation that has a significant impact on downstream processes and, ultimately, the quality of the final products. The development of a...Objective: In a chromatographic cycle, the adsorption process is a critical unit operation that has a significant impact on downstream processes and, ultimately, the quality of the final products. The development of a rapid method to determine the endpoints of adsorption processes in a large-scale manufacturing is of substantial importance for herbal medicine(HM) manufacturers.Methods: In this study, the adsorption of saponins on a macroporous resin column chromatograph, a critical unit operation in Panax notoginseng(Burkill) F.H.Chen injection manufacturing, was considered as an example. The evaluation results of in-line ultraviolet and visible spectra combined with various multivariate analysis methods, including the moving block standard deviation(MBSD), difference between the moving block average and the target spectrum(DMBA-TS), soft-independent modeling of class analogy(SIMCA), and partial least-squares discriminant analysis(PLS-DA), were compared.Results: MBSD was unsuitable for adsorption processes. The relative standard errors of prediction between the predicted and experimental endpoints were 13.2%, 4.67%, and 5.71% using DMBA-TS, SIMCA, and PLS-DA, respectively.Conclusions: Among the considered analysis methods, SIMCA and PLS-DA were more effective for endpoint determination. The results of this study provide a more comprehensive overview of the effectiveness of various multivariate analysis methods to facilitate the selection of the most suitable method. This study was also conducive to address the issues of the in-line detection of adsorption endpoints to guide practical HM manufacturing.展开更多
当前滴丸生产过程数字化、智能化水平较低,缺乏过程监控方法,难以有效控制滴丸的质量。因此,本文提出了一种基于激光检测技术和多变量数据分析(multivariate data analysis,MVDA)技术的滴丸滴制过程在线监控方法。该方法首先通过激光检...当前滴丸生产过程数字化、智能化水平较低,缺乏过程监控方法,难以有效控制滴丸的质量。因此,本文提出了一种基于激光检测技术和多变量数据分析(multivariate data analysis,MVDA)技术的滴丸滴制过程在线监控方法。该方法首先通过激光检测器高频采集滴丸滴制过程中下落液滴的宽度数据,其次基于宽度数据对每个液滴选取节点并提取特征指标,然后基于正常工艺条件下的特征数据集建立主成分分析(principal component analysis,PCA)模型,选择Hotelling’s T^(2)或DModX统计量判断滴制过程的液滴是否异常,并通过主成分得分图结合K近邻(K-nearest neighbor,KNN)算法对异常进行分类和诊断。本文以银杏叶滴丸的滴制过程为例,考察了该方法的可行性,结果表明所得到的模型对滴头阀门开度异常、药液温度异常、药液量异常具有较好的检测和诊断能力,该方法可为滴丸剂的工业生产提供一定的参考。展开更多
建立基于定量核磁共振(quantitative nuclear magnetic resonance,qNMR)技术的人参皂苷对照品质量评价方法。采用Bruker AvanceⅢ500 MHz核磁共振仪,配备5 mm BBO探头,采集定量氢谱,30°脉冲,弛豫延迟时间D_(1)为20 s,探头温度为303...建立基于定量核磁共振(quantitative nuclear magnetic resonance,qNMR)技术的人参皂苷对照品质量评价方法。采用Bruker AvanceⅢ500 MHz核磁共振仪,配备5 mm BBO探头,采集定量氢谱,30°脉冲,弛豫延迟时间D_(1)为20 s,探头温度为303 K,采样次数为32次。采用绝对定量法,选择高纯度的定量核磁共振用内标对苯二甲酸二甲酯,以灵敏度相对较好的甲基峰作为定量峰,结合线性拟合解卷积处理提高积分结果的准确性,建立了基于qNMR技术的人参皂苷对照品质量评价方法,并完成方法学验证。采用建立的qNMR对5种人参皂苷类对照品人参皂苷Rg_(1)、人参皂苷Re、人参皂苷Rb_(1)、人参皂苷Rd和三七皂苷R;进行质量评价研究,结果表明5种人参皂苷对照品qNMR测定值低于厂家提供的HPLC归一化含量。该方法可以保障人参皂苷对照品的质量,同时也为相关中药材及其制剂质量评价的准确性提供有力支持。基于qNMR技术的中药对照品质量评价方法简单、快捷、结果准确,值得推广用于中药对照品的质量值定量测定。展开更多
基金supported by the National Natural Science Foundation of China(82104383)National S&T Major Project of China(2012ZX09101201-003)
文摘Objective: In a chromatographic cycle, the adsorption process is a critical unit operation that has a significant impact on downstream processes and, ultimately, the quality of the final products. The development of a rapid method to determine the endpoints of adsorption processes in a large-scale manufacturing is of substantial importance for herbal medicine(HM) manufacturers.Methods: In this study, the adsorption of saponins on a macroporous resin column chromatograph, a critical unit operation in Panax notoginseng(Burkill) F.H.Chen injection manufacturing, was considered as an example. The evaluation results of in-line ultraviolet and visible spectra combined with various multivariate analysis methods, including the moving block standard deviation(MBSD), difference between the moving block average and the target spectrum(DMBA-TS), soft-independent modeling of class analogy(SIMCA), and partial least-squares discriminant analysis(PLS-DA), were compared.Results: MBSD was unsuitable for adsorption processes. The relative standard errors of prediction between the predicted and experimental endpoints were 13.2%, 4.67%, and 5.71% using DMBA-TS, SIMCA, and PLS-DA, respectively.Conclusions: Among the considered analysis methods, SIMCA and PLS-DA were more effective for endpoint determination. The results of this study provide a more comprehensive overview of the effectiveness of various multivariate analysis methods to facilitate the selection of the most suitable method. This study was also conducive to address the issues of the in-line detection of adsorption endpoints to guide practical HM manufacturing.
文摘建立基于定量核磁共振(quantitative nuclear magnetic resonance,qNMR)技术的人参皂苷对照品质量评价方法。采用Bruker AvanceⅢ500 MHz核磁共振仪,配备5 mm BBO探头,采集定量氢谱,30°脉冲,弛豫延迟时间D_(1)为20 s,探头温度为303 K,采样次数为32次。采用绝对定量法,选择高纯度的定量核磁共振用内标对苯二甲酸二甲酯,以灵敏度相对较好的甲基峰作为定量峰,结合线性拟合解卷积处理提高积分结果的准确性,建立了基于qNMR技术的人参皂苷对照品质量评价方法,并完成方法学验证。采用建立的qNMR对5种人参皂苷类对照品人参皂苷Rg_(1)、人参皂苷Re、人参皂苷Rb_(1)、人参皂苷Rd和三七皂苷R;进行质量评价研究,结果表明5种人参皂苷对照品qNMR测定值低于厂家提供的HPLC归一化含量。该方法可以保障人参皂苷对照品的质量,同时也为相关中药材及其制剂质量评价的准确性提供有力支持。基于qNMR技术的中药对照品质量评价方法简单、快捷、结果准确,值得推广用于中药对照品的质量值定量测定。
