摘要
目的:建立和优选测定熊去氧胆酸软胶囊主药含量的方法。方法:分别采用高效液相色谱柱前衍生测定法(一法)和直接测定法(二法)。色谱柱为SHISEIDO CAPCELL PAK-C18柱,一法流动相为甲醇-0.1%磷酸(80:20,V/V),检测波长为254nm,柱温为40℃,流速为1.0ml/min,进样量为10μl;二法流动相为乙睛-0.001mol/L磷酸二氢钾溶液(磷酸调pH值为2.0,47:53,V/V),检测波长为210nm,柱温为35℃,流速为1.0ml/min,进样量为20μl。结果:一法和二法熊去氧胆酸检测质量浓度分别在0.03371～0.10112、0.8～3.2mg/ml范围内与峰面积积分值呈良好的线性关系(r=0.9998和0.9999);精密度、稳定性、重复性试验的RSD均≤1.5%;平均回收率分别为99.51%、101.40%,RSD分别为0.65%、0.69%(均n=9)。结论:两种方法均可满足检测要求,但直接测定法操作更简便,结果更准确、可靠,可作为熊去氧胆酸软胶囊的质量控制方法。
OBJECTIVE： To establish the method for the content determination of main components in Ursodeoxycholic acid soft capsules. METHODS： HPLC method was adopted： pre-column derivatization method （method 1） and direct determination （method 2）. The separation was performed on SHISEIDO CAPCALL PAK-C18 column; the condition of method 1： the rhobile phase consisted of methanol-0.1% phosphoric acid （80：20, V/V） at the flow rate of 1.0 ml/min; the detection wavelength was set at 254 nm and column temperature was 40 ℃. The condition of method 2 ： the mobile phase consisted of acetonitrile-0.001 mol/L potassium dihydrogen phosphate solution （pH adjusted to 2.0 with phosphoric acid, 47 ： 53, V/V） at the flow rate of 1.0 ml/min; the detection wavelength was set at 210 nm and column temperature was 35 ℃. RESULTS： The linear range of ursodeoxycholic ac- id was 0.033 71-0.101 12 mg/ml by method 1 （r=0.999 8） and 0.8-3.2 mg/ml by method 2 （r=0.999 9） ; RSDs of precision, stabili- ty and reproducibility tests were lower than and equal to 1.5% ; average recoveries were 99.51% （RSD=0.65% , n=9） and 101.40% （RSD=0.69%, n=9）. CONCLUSIONS： The two methods are in line with the requirements. The method 2 is simple and accurate, and can be used for quality control of Ursodeoxvcholic acid soft caosules.
出处
《中国药房》
CAS
CSCD
2013年第24期2287-2289,共3页
China Pharmacy
