摘要
目的建立测定鹅去氧胆酸原料药含量的高效液相色谱-蒸发光散射(HPLC-ELSD)法。方法采用十八烷基硅烷键合硅胶填充C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-甲醇-0.10%甲酸溶液(58∶10∶32,V/V/V),流速为1.0 m L/min,等度洗脱,柱温为30℃,380-ELSD检测器,漂移管温度为90℃,N2流速为2.6 L/min。结果鹅去氧胆酸质量浓度在1.0~100.5μg/m L范围内与峰面积线性关系良好,R2=0.9896(n=7);检测限(LOD,S/N=3)、定量限(LOQ,S/N=10)分别为0.45μg/m L,1.52μg/m L;平均回收率为99.22%,RSD为1.29%(n=9);熊去氧胆酸质量浓度在1.0~103.2μg/m L范围内与峰面积线性关系良好,R2=0.9944(n=7);LOD(S/N=3)和LOQ(S/N=10)分别为1.14μg/m L和3.79μg/m L;平均加样回收率为96.72%,RSD为3.97%(n=9)。结论该方法操作方便,重复性好,精密度高,准确性强,可有效控制鹅去氧胆酸原料药的质量。
Objective To establish a high performance liquid chromatography-evaporative light scattering detection(HPLC-ELSD)method for the content determination of chenodeoxycholic acid drugs.Methods The C18 column(250 mm×4.6 mm,5μm)was filled with octadecylsilane chemically bonded silica.The mobile phase was acetonitrile-methanol-0.1%formic acid(58∶10∶32,V/V/V),the flow rate was 1.0 m L/min(isocratic elution),the column temperature was 30℃,the detector was 380-ELSD,the temperature of drift tube was 90℃,the flow rate of N2 was 2.6 L/min.Results Chenodeoxycholic acid showed a good linear relationship within the range of 1.0-100.5μg/m L with the peak area,R^2=0.9896(n=7);the detection limit(LOD,S/N=3)and the quantitative limit(LOQ,S/N=10)were 0.45μg/m L,1.52μg/m L respectively;the average recovery rate was 99.22%,the RSD was 1.29%(n=9).Ursodeoxycholic acid showed a good linear relationship within the range of 1.0-103.2μg/m L with the peak area,R^2=0.9944(n=7);LOD(S/N=3)and LOQ(S/N=10)were 1.14μg/m L and 3.79μg/m L respectively;the average recovery rate was 96.72%,the RSD was 3.97%(n=9).Conclusion The method is convenient,reproducible,precise and accurate,which can effectively control the quality of chenodeoxycholic acid.
作者
蔡明
徐倩
乔金为
鲍学梅
韩岚
彭代银
CAI Ming;XU Qian;QIAO Jinwei;BAO Xuemei;HAN Lan;PENG Daiyin(Department of Pharmacy,The Second Affiliated Hospital,Anhui University of Chinese Medicine,Hefei,Anhui,China 230001;School of Pharmacy,Anhui University of Chinese Medicine,Hefei,Anhui,China 230012)
出处
《中国药业》
CAS
2020年第15期55-57,共3页
China Pharmaceuticals
基金
安徽省教育厅高校自然科学研究重点项目[KJ2017A277]。
关键词
鹅去氧胆酸
熊去氧胆酸
高效液相色谱-蒸发光散射法
含量测定
chenodeoxycholic acid
ursodeoxycholic acid
high performance liquid chromatography-evaporative light scattering detection
content determination
