目的:建立青阳参苷甲对照品的制备方法和含量测定,为质量标准的提高提供参考。方法:采用植物化学方法制备青阳参苷甲作为对照品,采用质谱、核磁共振等光谱法鉴定对照品的结构,采用面积归一化法测定了对照品含量,并建立高效液相色谱法测...目的:建立青阳参苷甲对照品的制备方法和含量测定,为质量标准的提高提供参考。方法:采用植物化学方法制备青阳参苷甲作为对照品,采用质谱、核磁共振等光谱法鉴定对照品的结构,采用面积归一化法测定了对照品含量,并建立高效液相色谱法测定青阳参及同属药材白前、白薇和徐长卿中青阳参苷甲的含量。采用Waters X Select C18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-水溶液(43∶57),流速1.0 m L·min^(-1);检测波长223 nm;柱温30℃;进样量10μL。结果:经过鉴定分离的青阳参苷甲纯度大于98%,可作为质量研究用对照品。青阳参苷甲质量浓度在5.62~224.8μg·mL^(-1)(r=0.9998,n=6)范围内线性关系良好,方法的平均回收率(n=6)为97.7%(RSD=1.4%)。白前、白薇和徐长卿中未检出青阳参苷甲,青阳参中青阳参苷甲含量在0.015%~0.070%。结论:青阳参苷甲是青阳参的特征成分,可作为该药材的定量指标。本文所建立的高效液相色谱法可作为青阳参药材质量标准中的含量测定方法。展开更多
According to the standard of GB/T1500.3-2008 and the guidelines of ISO/REMCO, the preparation of National Certified Reference Materials （CRMs） of active compounds was composed of the following two aspects： preparat...According to the standard of GB/T1500.3-2008 and the guidelines of ISO/REMCO, the preparation of National Certified Reference Materials （CRMs） of active compounds was composed of the following two aspects： preparation and certification. This paper presents an example of the preparation of biochanin A to illustrate the preparation of National CRMs of active compounds from natural products. Firstly, the target compound was extracted and purified from crude materials. Then, its chemical structure was identified by UV spectrum, IR spectrum, ESI-MS, and NMR. The purity of the compound was determined by HPLC with the area normalization method. The certified value assessed by comparing the purity values from six independent qualified laboratories and the value of uncertainty were given. Thermal analysis, residual solvent, homogeneity testing and stability testing was tested in the process.展开更多
文摘目的:建立青阳参苷甲对照品的制备方法和含量测定,为质量标准的提高提供参考。方法:采用植物化学方法制备青阳参苷甲作为对照品,采用质谱、核磁共振等光谱法鉴定对照品的结构,采用面积归一化法测定了对照品含量,并建立高效液相色谱法测定青阳参及同属药材白前、白薇和徐长卿中青阳参苷甲的含量。采用Waters X Select C18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-水溶液(43∶57),流速1.0 m L·min^(-1);检测波长223 nm;柱温30℃;进样量10μL。结果:经过鉴定分离的青阳参苷甲纯度大于98%,可作为质量研究用对照品。青阳参苷甲质量浓度在5.62~224.8μg·mL^(-1)(r=0.9998,n=6)范围内线性关系良好,方法的平均回收率(n=6)为97.7%(RSD=1.4%)。白前、白薇和徐长卿中未检出青阳参苷甲,青阳参中青阳参苷甲含量在0.015%~0.070%。结论:青阳参苷甲是青阳参的特征成分,可作为该药材的定量指标。本文所建立的高效液相色谱法可作为青阳参药材质量标准中的含量测定方法。
基金The Natural Science Foundation of China (20872083)the Key Science and Technology Program of Shandong Province and the State Key Laboratory of Crop Biology (2008kf05)
文摘According to the standard of GB/T1500.3-2008 and the guidelines of ISO/REMCO, the preparation of National Certified Reference Materials （CRMs） of active compounds was composed of the following two aspects： preparation and certification. This paper presents an example of the preparation of biochanin A to illustrate the preparation of National CRMs of active compounds from natural products. Firstly, the target compound was extracted and purified from crude materials. Then, its chemical structure was identified by UV spectrum, IR spectrum, ESI-MS, and NMR. The purity of the compound was determined by HPLC with the area normalization method. The certified value assessed by comparing the purity values from six independent qualified laboratories and the value of uncertainty were given. Thermal analysis, residual solvent, homogeneity testing and stability testing was tested in the process.
