摘要
目的:建立HPLC-ELSD法测定猪胆粉中甘氨猪去氧胆酸和甘氨鹅去氧胆酸的含量测定方法。方法:猪胆粉甲醇提取液采用Welch Ultimate Plus C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.1%甲酸溶液(40∶60)为流动相,流速为1.0 ml·min^(-1),检测器为奥泰ELSD 2000ES,漂移管温度为105℃,氮气流速为每分钟2.5 L。结果:甘氨猪去氧胆酸和甘氨鹅去氧胆酸分别在0.306~4.590μg(r=0.999 5)、0.280~4.194μg(r=0.999 4)范围内呈现良好的线性关系,其平均回收率分别为99.23%,100.37%,RSD分别为2.0%,1.8%(n=9)。结论:该方法结果准确,灵敏度高,重复性好,可用于猪胆粉的质量控制。
Objective : To establish a method for the simultaneous determination of glycohyodeoxycholic acid and glycochenodeoxy- cholic acid in pulvis fellis suis by HPLC-ELSD. Methods: The analysis of methanol extract of pulvis fellis suis was performed on a Welch Ultimate Plus C,8 ( 250 mm×4.6 mm,5μm) column, and the mobile phase consisted of acetonitrile and 0.1% formic acid ( 40 : 60). The flow rate was 1.0 ml min -1. Allteeh ELSD 2000ES was used as the detector, the drift tube temperature was 105℃ and the nitrogen flow rate was 2.5 L min -1. Results: Glycohyodeoxycholic acid and glycochenodeoxyeholic acid had good linear relation- ships within the range of 0. 306-4. 590 μg( r = 0.999 5 ) and 0. 280-4. 194 μg( r = 0. 999 4 ), respectively. The average recovery was 99.23 % with RSD of 2.0% and 100.37% with RSD of 1.8% (n = 9), respectively. Conclusion: The method is accurate, sensitive and repeatable, which can be used for the quality control of pulvis fellis suis.
出处
《中国药师》
CAS
2017年第8期1480-1482,共3页
China Pharmacist