清开灵软胶囊中胆酸和猪去氧胆酸的含量测定

HPLC-ELSD Determination of Cholic Acid and Hyodeoxycholic Acid Contents in Qingkailing Soft Capsule

目的建立清开灵软胶囊中胆酸和猪去氧胆酸的高效液相色谱-蒸发光散射(HPLC-ELSD)含量测定方法。方法采用ShiseidoCapcell MGⅡC18色谱柱(150 mm×4.6 mm,5μm),以甲醇-乙腈-0.5%冰醋酸溶液(49∶20∶31)为流动相,流速为1.0 mL/min,柱温为25℃,蒸发光散射检测器,漂移管温度为108℃,载气流速为2.8 L/min。结果胆酸和猪去氧胆酸的进样量分别在2.338～18.704μg(r=0.999 4)和2.018～16.141μg(r=0.999 5)范围内与各自的峰面积积分值呈良好的对数线性关系,平均回收率分别为98.51%和98.01%,RSD分别为0.74%和0.72%(n=9)。结论所用方法简便、准确、分离效果好,适用于该制剂的质量控制。

Objective To establish a determination method of cholic acid and hyodeoxycholic acid in Qingkailing Soft Capsule by HPLC- ELSD. Methods The chromatographic analysis were carried out on the Shiseido CAPCELL MG Ⅱ C18 column（150 mm× 4.6 mm, 5μm）witb the mobile phase of methanol- acetonitrile-0.5% glacial acetic acid（49：20：31）. The flow rate was 1.0 mL/min,and the column temperature was 25℃. The evaporative light-scattering detector was adopted. The drift tube temperature was set at 108℃ with the cartier gas flow rate of 2. 8 L/min. Results The linear ranges of eholic acid and hyodeoxycholic acid were 2. 338- 18. 704 μg（ r=0. 999 4）and 2. 018- 16. 141 μg（r =0. 999 5）,respectively. Their average recovery rates were 98.51% （RSD =0.74%, n =9） and 98.01% （RSD=0.72%, n=9）,respeetively. Conclusion The used method is simple and accurate with good separation effect, which is suitable for the quality control of Qingkailing Soft Capsule.