| 引用本文: | 靖雅,王丽敏,杜诗琦,李博,狄斌.HPLC测定他达拉非中的对映异构体和非对映异构体[J].中国现代应用药学,2017,34(1):89-93. |
| JING Ya,WANG Limin,DU Shiqi,LI Bo,DI Bin.Determination of Enantiomers and Diastereoisomers in Tadalafil by HPLC[J].Chin J Mod Appl Pharm(中国现代应用药学),2017,34(1):89-93. |
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| HPLC测定他达拉非中的对映异构体和非对映异构体 |
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靖雅1, 王丽敏1, 杜诗琦1, 李博1, 狄斌1,2
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1.中国药科大学, 药学院, 南京 210009;2.中国药科大学, 药物质量与安全预警教育部重点实验室, 南京 210009
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| 摘要: |
| 目的 建立他达拉非原料药中对映异构体和非对映异构体的定量分析方法。方法 采用CHIRALPAK-IC（250 mm×4.6 mm，5 μm）色谱柱，流动相为乙腈-水（40：60），流速为1.0 mL·min-1，检测波长为222 nm，柱温为30℃，进样量20 μL。加校正因子的自身稀释对照法计算异构体含量，其中异构体A、异构体B和异构体C的校正因子分别为1.22，1.07和1.25。结果 他达拉非及异构体A、异构体B和异构体C峰分离良好，分离度>1.5，异构体A、异构体B和异构体C分别在25.3~379.5，50.6~379.5，50.4~378.0 ng·mL-1内线性关系良好（r为0.997 3~0.998 7），加样回收率分别为107.5%，96.9%，98.5%（n=9），进样精密度RSD≤2%，重复性RSD分别为1.44%，1.64%和4.89%。检测限分别为12.7，25.3，25.2 ng·mL-1。3批样品中异构体A最高含量为0.018%，异构体B及异构体C均未超过检测限（<0.010%）。结论 该方法简单，准确，重复性好，可用于他达拉非原料药中对映异构体和非对映异构体的测定。 |
| 关键词: 他达拉非 对映异构体 非对映异构体 高效液相色谱法 手性色谱柱 |
| DOI：10.13748/j.cnki.issn1007-7693.2017.01.021 |
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| Determination of Enantiomers and Diastereoisomers in Tadalafil by HPLC |
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JING Ya1, WANG Limin1, DU Shiqi1, LI Bo1, DI Bin1,2
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1.College of Pharmacy, China Pharmaceutical University, Nanjing 210009, China;2.Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, China Pharmaceutical University, Nanjing 210009, China
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| Abstract: |
| OBJECTIVE To develop an HPLC method for the determination of enantiomers and diastereoisomers in tadalafil. METHODS A CHIRALPAK-IC column(250 mm×4.6 mm, 5 μm) was adopted. The mobile phase was acetonitrile-water(40:60) at the flow rate of 1.0 mL·min-1 and injection volume of 20 μL. The UV-detection wavelength was set at 222 nm with the column temperature of 30℃. The isomer contents were calculated by self contrast method with the correction factor, and the correction factor of isomer A, isomer B and isomer C were 1.22, 1.07 and 1.25 respectively. RESULTS Calibration curves were found to be linear in the ranges of 25.3-379.5 ng·mL-1 for isomer A, 50.6-379.5 ng·mL-1 for isomer B and 50.4-378.0 ng·mL-1 for isomer C(r=0.997 3-0.998 7). The average recovery(n=9) of isomer A, isomer B, and isomer C were 107.5%, 96.9%, and 98.5%, respectively. RSD of repeatability was 1.44%, 1.64% and 4.89% respectively, and the RSD of sampling precision was ≤2%. The LOD of isomer A, isomer B and isomer C were 12.7, 25.3, 25.2 ng·mL-1. Isomer B and C were not detected (<0.01% of tadalafil) and the content of isomer A was up to 0.018% in 3 batches of samples. CONCLUSION The method is simple, accurate and reproducible. It can be reliable for the quality control of enantiomers and diastereoisomers of tadalafil. |
| Key words: tadalafil enantiomers diastereoisomers HPLC chiral columns |
