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  

Determination of the major bile acids in pig bile powder by HPLC-ELSD and chemometric analysis of the whole chromatographic profiles

作　　者：石岩[1] 耿颖[1] 郑天骄[1,2] 魏锋[1] 林瑞超[3,4] 马双成[1] 

机构地区：[1]中国食品药品检定研究院,北京100050 [2]中国药科大学,南京211198 [3]沈阳药科大学中药学院,沈阳110016 [4]北京中医药大学中药学院,北京100102

出　　处：《药物分析杂志》2017年第2期283-289,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：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)

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-C_(18)色谱柱(4.6 mm×250 mm,5μm),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 m L·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。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 m L·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）.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.

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 

分 类 号：R917[医药卫生—药物分析学]