HPLC法测定盐酸莫西沙星中R-异构体含量

目的: 建立HPLC法对盐酸莫西沙星S-和R-异构体进行拆分并测定其中R-异构体含量。 方法: 采用AD-H手性柱(DAICEL CHIRALPAK,250 mm×4.6 mm,5 μm),流动相为正己烷-异丙醇-二乙胺-乙酸(85∶ 15∶ 0.2∶ 0.1),流速1.0 mL·min^-1,柱温35 ℃,检测波长293 nm;进样量10 μL。 结果: 盐酸莫西沙星异构体之间的分离度为3.4,R-异构体的线性范围为0.54～5.40 μg·mL^-1(r=0.9995),检测限为1.1 ng,平均回收率(n=9)为99.2%。 结论: 该方法操作简便,结果准确,可用于盐酸莫西沙星中R-异构体含量测定。

Objective: To establish an HPLC method for enantioseparation of S-and R-moxifloxacin hydrochloride and assay of the R-isomer. Methods: The separation was performed on an AD-H chiral column (DAICEL CHIRALPAK, 250 mm×4.6 mm, 5 μm). The mobile phase was n-hexane-iso-propylalcohol-diethy lamine-acetic acid(85∶ 15∶ 0.2∶ 0.1) at the flow rate of 1.0 mL·min^-1; The column temperature was 35 ℃, and the detection wavelength was set at 293 nm; The injection volume was 10 μL. Results: The resolution of the isomer was 3.4, the linear range of the R-isomer was 0.54-5.40 μg·mL^-1(r=0.9995), the detection limit was 1.1 ng and the average recovery(n=9) was 99.2%. Conclusion: The method is simple and accurate, and can be used for assay of R-isomer in moxifloxacin hydrochloride.

[1] JIANG Chao(江超),ZHOU Yi-sui(周宜遂).Graphical synthetic routes of moxifloxacin(莫西沙星合成路线图解).Chin J Pharm(中国医药工业杂志),2009,40(5):393
[2] ZHANG Zhi-wei(张志伟),LI Jin-wei(李金伟),DONG Gen-shan(董根山).Preparation and quality control of moxifloxacin hydrochloride effervescent tablet(盐酸莫西沙星泡腾片的制备及质量控制).China Pharm(中国药房),2007,18(19):1486
[3] USP 32-NF 27.2009.Suppl(2):4264
[4] Cruz LA,Hall R.Enantiomeric purity assay of moxifloxacin hydrochloride by capillary electrophoresis.J Pharm Biomed Anal,2005,38(1):8
[5] Ravikumar M,Varma MS,Raju TS,et al.Enantiomeric separation of moxifloxacin and its (R,R)-isomer by ligand-exchange chiral chromatography.Chromatographia,2009,69(1/2):85
[6] CHEN Ying(陈英).Suggestion on the system suitability test of HPLC in related substances(对HPLC法有关物质系统适用性建立的体会和建议).Drug Stand China(中国药品标准),2010,11(5):323
[7] XIE Mu-feng(谢沐风).How to establish an HPLC method for determination of related substances in drugs(如何建立高效液相色谱法测定有关物质的方法).Chin J Pharm(中国医药工业杂志),2007,38(1):45
[8] EP 6.0.2007.2451