| 王仁,纪学敏,黄蓉,刘常悦.3α-羟基-7-氧代-胆烷酸有关物质分析方法的建立[J].中国药品标准,2017,18(4):283-287 |
| 3α-羟基-7-氧代-胆烷酸有关物质分析方法的建立 |
| Study on Determination Method for Related Substances of (E)-3α-hydroxy-6-ethylidene-7-keto-5β-cholan-24-oic acidRen Wang,Xue min Ji(Hangzhou Minsheng Institute for Pharma Research Co．,Ltd．,Hangzhou 311121) |
| 投稿时间：2017-06-26 修订日期：2017-07-31 |
| DOI： |
| 中文关键词: 奥贝胆酸 3α-羟基-7-氧代-胆烷酸 有关物质 高效液相色谱法 |
| 英文关键词: Obeticholic Acid (E)-3α-hydroxy-6-ethylidene-7-keto-5β-cholan-24-oic acid Related substances HPLC |
| 基金项目: |
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| 摘要点击次数: 517 |
| 全文下载次数: 126 |
| 中文摘要: |
| 目的：建立3α-羟基-7-氧代-胆烷酸有关物质的分析方法。方法：以碳十八烷基键合硅胶柱为填充剂,以0.05%的磷酸水溶液和乙腈为流动相,流速为1.0 mL/min,检测波长为202nm。 结果：3α-羟基-7-氧代-胆烷酸样品溶液的色谱图中主峰与已知杂质之间和各已知杂质之间均能有效分离,3α-羟基-7-氧代-胆烷酸、杂质01、杂质04、杂质05和杂质06-A分别在1.00～24.97 μg.mL-1(r =0.9999),1.00～50.05 μg.mL-1(r =0.9999),0.75～25.04 μg.mL-1(r =0.9999),1.01～5.02 μg.mL-1(r =0.9998),1.00～9.98 μg.mL-1(r =0.9999)的浓度范围内与峰面积成良好的线性关系；检测限分别为12.5ng,12.5ng,10ng,12.5ng,12.5ng。 |
| 英文摘要: |
| Objective： To establish a method for determining related substances of (E)-3α-hydroxy-6-ethylidene-7-keto-5β-cholan-24-oic acid Method： HPLC was adopted and the separation was performed on a C18 column with 0.05% phosphoric acid aqueous solution and acetonitrile as mobile phase. the flow rate wes 1.0 ml/min,the detection wavelength was 202 nm. Result： (E)-3α-hydroxy-6-ethylidene-7-keto-5β-cholan-24-oic acid chromatographic peaks could be well separated from the identified impurity, The identified impurities could also be well separated；(E)-3α-hydroxy-6-ethylidene-7-keto-5β-cholan-24-oic acid and impurity 01、04、05、06-A showed agood linear relationship within therange of 1.00～24.97 μg.mL-1(r =0.9999),1.00～50.05 μg.mL-1(r =0.9999),0.75～25.04 μg.mL-1(r =0.9999),1.01～5.02 μg.mL-1(r =0.9998),1.00～9.98 μg.mL-1(r =0.9999)；the detection limit was12.5ng,12.5ng,10ng,12.5ng,12.5ng.Conclusion： It is proved that the method is simple and feasible, and its specificity, sensitivity, linearity and precision are good, and it is suitable for the determination of related substances in this product. |
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