HPLC法手性柱检测恩曲他滨的对映体

HPLC determination of emtricitabine enantiomer by chirality column

目的:建立恩曲他滨有关物质及手性对映体的检测方法。方法:有关物质:采用 SHIMADZU VP-ODS 色谱柱(150 mm×4.6 mm,5μm);流动相为0.02 mol·L^(-1)醋酸铵缓冲溶液(醋酸铵1.54 g,加水1000 mL,冰醋酸调节 pH 至3.85～3.95)-甲醇(85:15);流速:1 mL·min^(-1),检测波长280 nm。手性对映体:采用 CHIROBIOTIC TAG^(TM)手性色谱柱(大环糖肽,5μm,250 mm×4.6 mm),流动相为甲醇-三乙胺-冰醋酸(100:3.5:2.4);流速:1 mL·min^(-1);检测波长280 nm。结果:有关物质检查中,检测限为0.1443 ng,恩曲他滨经强酸、强碱、高温、氧化等剧烈条件破坏,所产生的降解产物峰与恩曲他滨峰能很好地分离。手性对映体检查中,检测限为0.45 ng,手性对映体的分离度为1.6。结论:本恩曲他宾有关物质及手性对映体的检测方法简便快速,灵敏度高,准确可靠。

Objective：To establish the method for determining the related substance and its chirality enantiomer of emtricitabine. Method：related substance：Use SHIMADZU VP- ODS chromatographic column （150 mm × 4. 6 mm, 5 μm） ;flow liquid is 0. 02 mol·L^-1 ammonium acetate buffer solution （ammonium acetate 1.54 g, adding water to 1000 mL,using acetate to regulate pH value to 3. 85 -3.95） -methanol（85： 15） ;flow rate：1 mL ·min^-1 ,determination wavelength is 280 nm. Chirality drug：Use CHIROBIOTIC TAGTM chirality chromagraphic column （macrocyclic glycopeptide,5 μm, 250 mm × 4. 6 mm） ;flow liquid is methanol - triethylamine - acetic acid （ 100： 3.5： 2. 4） ;flow rate： 1 mL ·min^-1, determination wavelength is 280 nm. Results：The detection limits was 0. 1443 ng for related substance. The degradation peaks produced by destroy emtricitabine with strong acid, alkali, high tempera- ture and oxidation respectively could be well separated from that of emtricitabine by this method. The limits was 0. 45 ng and the resolution was 1.6 for chirality enantiomer. Conclusion：This is a rapid accurate, reliable and sensitive method for detecting related substance and chirality enantiomer of emtricitabine.