PDF《石岩 1,耿颖 1,郑天骄 1,》

・283・ 标准研讨 猪胆粉 HPLC-ELSD 全轮廓谱图主要胆汁酸测定及化学计量学分析 * 石岩

1 , 耿颖

1 , 郑天骄 1,

4 , 魏锋

1 , 林瑞超 2,

3 , 马双成

1 (1.

中国食品药品检定研究院, 北京 100050;

2. 沈阳药科大学中药学院, 沈阳 110016;

3. 北京中医药大学中药学院, 北京 100102;

4. 中国药科大学, 南京 211198) 摘要 目的: 建立测定猪胆粉中主要胆汁酸类成分的 HPLS-ELSD 法, 并对样品的全轮廓色谱图进行化学 计量学分析.方法: 采用 SB-C18 色谱柱 (4.6 mm*250 mm,

5 μm) , 柱温为

40 ℃, 流动相为 0.2% 甲酸水溶 液-乙腈, 梯度洗脱, 流速 1.0 mL・min-1 ;

ELSD 漂移管温度为

110 ℃, 氮气流量为 2.8 L・h-1 , 增益为 1.使用COW 法校正样品的色谱峰, 并对数据进行聚类分析和主成分分析.结果: 有2批样品未检出甘氨猪去 氧胆酸和甘氨鹅去氧胆酸, 另外

20 批样品的甘氨猪去氧胆酸和甘氨鹅去氧胆酸的含量分别在 6.4%~36.5% 和4.5%~27.0% 之间.化学计量学分析结果表明, 自制样品与对照药材图谱更接近, 而与市售样品差异较 大.结论: 该法适合从定性和定量的角度对猪胆粉进行质量评价与控制. 关键词: 动物药;

猪胆粉;

胆汁酸;

甘氨猪去氧胆酸;

甘氨鹅去氧胆酸;

高效液相色谱;

蒸发光散射检测器;

聚类分析;

主成分分析 中图分类号: R

917 文献标识码: A 文章编号: 0254-1793 (2017) 00-0283-07 doi: 10.16155/j.0254-1793.2017.02.14 Determination of the major bile acids in pig bile powder by HPLC-ELSD and chemometric analysis of the whole chromatographic profiles* SHIYan1 , GENGYing1 , ZHENGTian-jiao1,

4 , WEIFeng1 , LINRui-chao2,

3 , MAShuang-cheng1 (1.National Institutes for Food and Drug Control, Beijing l00050, China;

2.School of Traditional Chinese Materia Medica, Shenyang Pharmaceutical University, Shenyang 110016, China;

3.School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 100102, China;

4.China Pharmaceutical University, Nanjing 211198, China) Abstract Objective: To establish a method for determination of the major bile acids in pig bile powder and its chemometric analysis of the whole chromatographic profiles. Methods: This analysis was performed at

40 ℃ on a SB- C18 column (4.6 mm*250 mm,

5 μm) . The mobile phase consisted of 0.2% formic acid solution and acetonitrile as a linear gradient elution and the flow rate was 1.0 mL・min-1 . An ELSD was used with a nitrogen flow-rate of 2.8 L・h-1 at a drift tube temperature of

110 ℃ and the gain was 1. The data of these chromatograms were processed by COW method and analyzed by hierarchical clustering analysis (HCA) and principle component analysis (PCA) . * 国家十二五 重大新药创制 专项课题――中药质量安全检测和风险控制技术平台 (2014ZX09304307-002) 第一作者 Tel: (010) 67095995;

E-mail: [email protected] ・284・ Results: Glycohyodeoxycholic acid and glycochenodeoxycholic acid were not detected in two batches samples from market. The content ranges of glycohyodeoxycholic acid and glycochenodeoxycholic acid in the other samples were 6.4%-36.5% and 4.5%-27.0%, respectively. The chemometrics showed that self-prepared samples were closer with reference medicinal material than market samples. Conclusion: Simultaneous qualitative and quantitative methods are suitable for the quality evaluation and the quality control of pig bile powder. Keywords: animal medicine;