HPLC-ELSD用于羊胆粉中胆酸及甘氨胆酸的测定研究

目的研究建立准确度高、重复性好的测定羊胆粉中胆酸和甘氨胆酸的方法。方法采用高效液相色谱仪与蒸发光散射检测器联用技术对羊胆粉进行测定。色谱条件：色谱柱Wondasil C18（4.6mm×250mm,5μm）;柱温25℃;流速1.0mL·min-1;ELSD检测器氮气流速2.3L·min-1,漂移管温度110℃;流动相A为0.2%甲酸溶液,流动相B为乙腈,梯度洗脱（0-7min,5%B;7-15min,5%→80%B）。结果同时测定了羊胆粉中的胆酸和甘氨胆酸含量,胆酸和甘氨胆酸进样量分别在0.163-0.817μg和0.160-0.801μg之间线性关系良好,平均回收率（n=6）分别为103.2%（RSD=1.7%）和101.2%（RSD=1.3%）。结论该法操作简便,测定准确,可用于羊胆粉的质量评价与控制。

Study on Determination of Cholic Acid and Glycocholic Acid from Capra Ovis Fellis Pulvis by HPLC-ELSD

Objective To establish a method for the determination of cholic acid and glycocholic acid in Capra Ovis Fellis Pulvis. Methods An HPLC-ELSD method was established for this determination. Chromatography was performed on a Wondasil C18 （4.6 mmX250 mm, 5 μm） column at 25 ℃. An evaporative light-scattering detector （ELSD） was used with the gas flow rate of 2.3 L . min-1 , and the drift tube temperature at 110 ℃. The mobile phase composition was 0.2% aqueous formic acid （A） and acetonitrile （B） with a flow rate of 1.0 mL . min-1 using a gradient elution （0-7 min, 5%B; 7-15 min, 5 -80 . B）. Results Cholic acid and glycocholic acid can be determined simultaneously. The linear ranges of eholic acid and glycocholic acid were 0. 163-0. 817 〉g and 0. 160-0. 801 /,g, and the average recoveries （n：6） were 103.2% （RSD：I. 7%） and 101.2o//00 （RSD=1. 3）. Conclusion The method is simple and accurate. It can be used for the quality evaluation and control of Capra Ovis Fellis Pulvis.