近红外漫反射光谱法快速测定苦参和白土苓药材中多指标成分的含量

doi:10.3964/j.issn.1000-0593(2014)10-2652-05

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摘要：建立近红外光谱(near infrared spectroscopy, NIRS)法快速测定复方苦参注射液原料药材苦参和白土苓中多指标成分含量的方法，探讨其在中成药原料质量保障系统中的应用可行性。以HPLC法测定苦参中氧化苦参碱、氧化槐果碱、苦参碱和槐果碱以及白土苓中大泽米苷的含量为对照值;采用近红外漫反射模式采集样品光谱，比较不同建模波段及光谱预处理方法的建模效果，优选出最佳建模参数;采用偏最小二乘法分别建立白土苓中大泽米苷和苦参中氧化苦参碱与苦参碱总量、槐果碱与氧化槐果碱总量的近红外定量分析模型，并对模型进行评价。结果显示，HPLC测定的88批白土苓中大泽米苷和75批苦参中氧化苦参碱与苦参碱总量、槐果碱与氧化槐果碱总量分别0.36～12.88，8.87～66.31和2.30～15.11 mg·g^-1。所建立的三组指标成分的NIRS定量校正模型性能良好，各模型校正集内部交叉验证R²为0.902 5, 0.949 1, 0.913 7，RMSECV为0.961, 2.45, 0.724 mg·g^-1;验证集外部验证R² 0.981 7，0.982 6，0.960 9，RMSEP为0.693，2.27，0.658 mg·g^-1。建立了快速定量苦参和白土苓中多指标成分的含量的近红外分析方法，所建立的定量分析模型能够满足复方苦参注射液大生产对大批量原料样品化学信息快速获取的需求。

关键词：近红外漫反射光谱;苦参;白土苓;大泽米苷;苦参生物碱;快速测定

Abstract：A rapid NIRS method for determination of macrozamin in Heterosmilacis japonicae rhizoma (HJR), and the total content of oxymatrine and matrine (OMT+MT) as well as the total content of oxysophocarpine and sophocarpine (OSC+SC) in sophorae flavescens radix (SFR) was developed to explore the application feasibility of NIRS for the quality assurance system of Chinese patent drugs. The contents of macrozamin in HJR samples, and OMT+MT and OSC+SC in SFR samples were determined by HPLC as reference values. The NIR spectra of the samples were measured in a diffused reflection mode. The different characteristic wavebands and pretreatment methods were optimized. The quantitative calibration models between the NIR spectra and the content reference values of marker components in HJR and SFR samples, were established with partial least square method, and further optimized through the cross validation and external validation. The contents of macrozamin in 88 batches of HJR samples were over the range of 0.36~12.88 mg·g^-1. The total contents of OMT+MT and OSC+SC in 75 batches of SFR samples were over the range of 8.87~66.31 and 2.30~15.11 mg·g^-1, respectively. The performance of the final models for macrozamin, OMT+MT and OSC+SC was evaluated well according to correlation coefficients (r), root mean square error of cross-validation (RMSECV) and root mean square error of prediction (RMSEP). The R² values of the cross-validation for macrozamin, OMT+MT and OSC+SC were 0.902 5, 0.949 1 and 0.913 7, and those of RMSECV were 0.961, 2.45 and 0.724 mg·g^-1 respectively. The R² values of external validation for the three models were 0.981 7, 0.982 6 and 0.960 9, and those of RMSEP were 0.693, 2.27 and 0.658 mg·g^-1, respectively. This is the first report on rapid determination of macrozamin in Heterosmilacis japonicae rhizoma, and oxymatrine, matrine, oxysophocarpine and sophocarpine in sophorae flavescens radix by NIRS method. The presented method can fulfill the requirement of rapid acquirement of chemical information of raw medicinal materials prior the manufacturing of compound Kushen injection.

Key words：Near infrared diffused reflectance spectroscopy;Sophorae flavescens radix;Heterosmilacis japonicae rhizoma;Macrozamin;Kushen alkaloids;Rapid determination

收稿日期: 2014-05-08 修订日期: 2014-07-22

中图分类号:

O657.3

通讯作者: 高慧敏，王智民 E-mail: huimin_gao@126.com;zhmw123@263.net

引用本文:

赵凤春，万楷杨，刘晓谦，张启伟，高慧敏^*，王智民^*. 近红外漫反射光谱法快速测定苦参和白土苓药材中多指标成分的含量[J]. 光谱学与光谱分析, 2014, 34(10): 2652-2656.
ZHAO Feng-chun, WAN Kai-yang, LIU Xiao-qian, ZHANG Qi-wei, GAO Hui-min^*, WANG Zhi-min^*. Rapid Determination of the Multi-Marker Ingredients in Heterosmilacis Japonicae Rhizoma and Sophorae Flavescentis Radix with Near-Infrared Diffused Reflection Spectroscopy. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2014, 34(10): 2652-2656.

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