摘要
目的建立HPLC-ELSD同时测定6种胆酸类成分的分析方法,并比较两种牛黄中胆酸类成分的含量。方法采用HPLC-ELSD法,以甲醇和0.1%的醋酸水溶液为流动相,梯度洗脱,流速1.0 mL.min-1,漂移管温度85℃,气体流速2.0 L.min-1。结果石胆酸、熊去氧胆酸、猪去氧胆酸、胆酸、鹅去氧胆酸、去氧胆酸线性范围分别为6.05～96.65,5.37～85.85,4.69～75,6.77～108.35,5.32～85,5.42～86.65 mg.L-1;检测限分别为0.75,0.74,0.65,0.63,0.63,1.05 ng.mL-1;加标回收率分别为99.43%,101.2%,100.4%,102.0%,101.7%,100.0%。结论本法操作简便,结果准确,重现性好,可用于牛黄及其各种制剂中胆酸类成分的质量控制。
OBJECTIVE To establish a HPLC-ELSD method for the determination for the content of six cholic acid derivatives and comparison of the content in two kinds of calculus bovis.METHODS A HPLC analysis was carried out on a Diamonsil C18 column（4.6 mm×250 mm,5 μm）with the mobile phase consisting of methanol（A）-0.1% acetic acid aqueous solution in gradient mode.The flow rate was 1.0 mL·min-1.The temperature of drift tube was 85 ℃,and the flow rate of gas was 2.0 L·min^-1.RESULTS The linearities of litho cholic acid,ursodeoxycholic acid,hyodeoxycholic acid,cholic acid,chenodeoxy cholic acid and deoxycholic acid were in the range of 6.05-96.65,5.37-85.85,4.69-75,6.77-108.35,5.32-85 and 5.42-86.65 mg·L^-1.The limits of detection were 0.75,0.74,0.65,0.63,0.63 and 1.05 ng·mL^-1.The average recoveries were 99.43%,101.2%,100.4%,102.0%,101.7% and 100.0%.CONCLUSION The method was simple,accurate and reproducibility,and can be used for the quality control of cholic acid derivatives in calculus bovis and various preparations of calculus bovis.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2010年第8期626-629,共4页
Chinese Pharmaceutical Journal
