Shi Yan, Zheng Tian-Jiao, Wei Feng, Lin Rui-Chao, Ma Shuang-Cheng
National Institutes for Food and Drug Control, Beijing 100050, China.
School of Traditional Chinese Materia Medica, Shenyang Pharmaceutical University, Shenyang 110016, China.
Zhongguo Zhong Yao Za Zhi. 2016 Jul;41(13):2487-2492. doi: 10.4268/cjcmm20161319.
An HPLC-ELSD method with good specificity and good accuracy was used for the studies of fingerprint and quantification of multi-components for cattle bile powder. The chromatographic analysis was carried out on a Phenomenex Gemini C₁₈ column (4.6 mm×250 mm, 5 μm) with a column temperature of 40 ℃ and a liquid flow-rate of 1.0 mL•min⁻¹ using 10 mmol ammonium acetate solution and acetonitrile as the mobile phase with a linear gradient. An ELSD was used with a nitrogen flow-rate of 2.8 L•h⁻¹, at a drift tube temperature of 110 ℃. The average contents of glycocholic acid, glycodeoxycholic acid, taurocholic acid, taurodeoxycholic acid were (25.2±17.0)%, (4.1±3.4)%, (24.5±20.0)% and (5.2±3.8)% respectively, and the total content of the four bile acids was (59.0±26.0)%. Beyond that, the preprocessing and pattern recognition analysis of the chromatographic fingerprints of samples were applied with chemometric method. The results of this chemometric analysis indicated that the samples from market and self-made samples were different signally, and four regions were noteworthy due to their great impact with poor chromatographic signal. All in one, because this HPLC-ELSD method was simple and accurate, it was suitable for the quality assessment and quality control of cattle bile powder and could be the technological base for its standard perfection.
采用一种具有良好特异性和准确性的高效液相色谱 - 蒸发光散射检测法对牛胆粉进行指纹图谱及多成分定量研究。色谱分析在Phenomenex Gemini C₁₈柱（4.6 mm×250 mm，5 μm）上进行，柱温40℃，以10 mmol醋酸铵溶液和乙腈为流动相，流速1.0 mL•min⁻¹，采用线性梯度洗脱。使用蒸发光散射检测器，氮气流量为2.8 L•h⁻¹，漂移管温度为110℃。甘氨胆酸、甘氨脱氧胆酸、牛磺胆酸、牛磺脱氧胆酸的平均含量分别为(25.2±17.0)%、(4.1±3.4)%、(24.5±20.0)%和(5.2±3.8)%，四种胆汁酸的总含量为(59.0±26.0)%。此外，采用化学计量学方法对样品色谱指纹图谱进行预处理和模式识别分析。化学计量学分析结果表明，市售样品和自制样品信号不同，且有四个区域因色谱信号差影响较大而值得关注。总之，由于该高效液相色谱 - 蒸发光散射检测法简单准确，适用于牛胆粉的质量评价和质量控制，可为其标准完善提供技术依据。
