摘要
中药的生产过程主要凭经验来控制,缺乏有效的在线监测技术,直接影响其质量。近红外光谱技术作为一种在线监测技术,已在众多领域得到广泛应用。本课题研究了近红外光谱技术应用于上市品种三七三醇皂苷和三七通舒胶囊生产过程的质量控制,主要内容包括：
1、对三七三醇皂苷进行了HPLC含量测定方法学考察,为近红外定量模型的建立奠定了基础。经系统适用性试验及方法学考察,专属性、线性、重复性、加样回收、精密度、稳定性均达到相应的要求。
2、以人参皂苷Rg1、人参皂苷Re、三七皂苷R1、三七三醇皂苷(PTS)的HPLC测定值为对照,建立了三七三醇皂苷渗漉提取过程的近红外光谱快速测定模型。渗漉过程人参皂苷Rg1定量模型校正集标准偏差(RMSECV)为0.798、相关系数(R2)为0.9682,预测集标准偏差(RMSEP)为1.1097、相关系数(R2)为0.9831；人参皂苷Re定量模型校正集标准偏差(RMSECV)为0.0945、相关系数(R2)为0.9681,预测集标准偏差(RMSEP)为0.4916、相关系数(R2)为0.9198；三七皂苷R1定量模型校正集标准偏差(RMSECV)为0.259、相关系数(R2)为0.9626,预测集标准偏差(RMSEP)为0.3899、相关系数(R2)为0.9661；三七三醇皂苷(PTS)定量模型校正集标准偏差(RMSECV)为1.1、相关系数(R2)为0.9714,预测集标准偏差(RMSEP)为0.9769、相关系数(R2)为1.8713。结果表明,本方法可用于三七三醇皂苷渗漉提取过程分析及质量控制。
3、以人参皂苷Rg1、人参皂苷Re、三七皂苷R1、三七三醇皂苷(PTS)的HPLC测定值和洗脱液乙醇浓度为对照,建立了三七三醇皂苷大孔吸附树脂纯化过程的近红外光谱快速测定模型。大孔吸附树脂纯化过程人参皂苷Rg1定量模型校正集标准偏差(RMSECV)为0.952、相关系数(R2)为0.9858,预测集标准偏差(RMSEP)为1.13、相关系数(R2)为0.9884；人参皂苷Re定量模型校正集标准偏差(RMSECV)为0.106、相关系数(R2)为0.9787,预测集标准偏差(RMSEP)为0.121、相关系数(R2)为0.9898；三七皂苷R1定量模型校正集标准偏差(RMSECV)为0.214、相关系数(R2)为0.9793,预测集标准偏差(RMSEP)为0.381、相关系数(R2)为0.9709；三七三醇皂苷(PTS)定量模型校正集标准偏差(RMSECV)为0.921、相关系数(R2)为0.9874,预测集标准偏差(RMSEP)为1.52、相关系数(R2)为0.9907；洗脱液乙醇浓度测定模型校正集标准偏差(RMSECV)为0.954、相关系数(R2)为0.9975,预测集标准偏差(RMSEP)为1.176、相关系数(R2)为0.9985。结果表明,本方法可用于三七三醇皂苷大孔吸附树脂纯化过程分析及质量控制。
4、建立了运用近红外光谱判断三七通舒胶囊生产过程中间体均匀度的方法,能有效监测三七通舒胶囊混合工艺过程中间体的均匀度,可应用于三七通舒胶囊生产过程的质量控制。
The manuacturing process of Traditional Chinese medicine(TCM) hans been mainly monitored with experience, experience. The absence of effective on-line monitoring techniques will affect the quality of TCM. This project is a research on near-infrared spectroscopy applied to quality control of the production process of protopanaxatriol saponin(PTS) and SanQiTongShu capsule.
1.This article studied HPLC method validation for quantitative analysis of the PTS, it laid a good foundation for Near-infrared quantitative model. In this study,specificity, linearity, repeatability, recovery, precision, and stability all meet the requirements.
2.Reference measurements of ginsenoside-Rg1,ginsenoside-Re and notoginsenoside-R1 were performed by HPLC,the study established the near infrared spectroscopy model for rapid determination in the extraction process of PTS by percolation. In the models,RMSECV for ginsenoside-Rg1 is 0.798, R2 is 0.9682, RMSEP for ginsenoside-Rg1 is 1.1097, R2 is 0.9831; RMSECV for ginsenoside-Re is 0.0945, R2 is 0.9681, RMSEP for ginsenoside-Re is 0.4916, R2is 0.9198; RMSECV for notoginsenoside-R1 is 0.259, R2is 0.9626, RMSEP for notoginsenoside-R1 is 0.3899, R2 is 0.9661; RMSEC for PTS is 1.1, R2is 0.9714, RMSEP for PTS is 0.9769, R2 is 1.8713. The results show that the present method can be applied for process analysis and quality control of protopanaxatriol saponin manufacturing process of extraction by percolation.
3.Reference measurements of ginsenoside-Rg1,ginsenoside-Re and notoginsenoside-R1 were performed by HPLC,and the ethanol content of Eluent,the study established the near infrared spectroscopy model for rapid determination in the purification process of PTS by macroporous resin. In the models,RMSECV for ginsenoside-Rg1 is 0.952, R2 is 0.9858, RMSEP for ginsenoside-Rg1 is 1.13, R2 is 0.9884; RMSECV for ginsenoside-Re is 0.106, R2 is 0.9787, RMSEP for ginsenoside-Re is 0.121, R2 is 0.9898; RMSECV for notoginsenoside-R1 is 0.214, R2 is 0.9793, RMSEP for notoginsenoside-R1 is 0.381, R2 is 0.9709; RMSECV for PTS is 0.921, R2 is 0.9874, RMSEP for PTS is 1.52, R2 is 0.9907. The results show that the present method can be applied for process analysis and quality control of protopanaxatriol saponin manufacturing process of purification by macroporous resin.
4.The study established the method for controlling the uniformity of the Intermediates of SanQiTongShu capsule by near-infrared spectroscopy,which can effectively monitor the uniformity of the intermediate of the mixing process of SanQiTongShu capsule.The method can be applied for process analysis and quality control of SanQiTongShu capsule manufacturing process.
引文
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