盐酸非那沙星原料药中RR型异构体的HPLC法测定.PDF

现代药物与临床 Drugs Clinic 第 30 卷 第 7 期 2015 年 7 月 ·805 · 盐酸非那沙星原料药中R,R 型异构体的 HPLC 法测定 1 2 1* 王 冬 ，李晓博 ，王 晨 1. 天津医科大学肿瘤医院 国家肿瘤临床医学研究中心 天津市肿瘤防治重点实验室，天津 300060 2. 天津医科大学 药学院，天津 300070 摘 要：目的 建立盐酸非那沙星原料药中 R,R 型异构体的 HPLC 测定方法。方法 采用 Chiralpak AY-H 手性色谱柱（250 mm ×4.6 mm ，5 µm ）；正庚烷–异丙醇–二乙胺（75 ∶25 ∶0.1 ）为流动相；体积流量为 1.0 mL/min；柱温35 ℃；检测波 长为 295 nm ；进样量 10 µL。结果 盐酸非那沙星在 101.2～813.1 ng/mL、R,R 型异构体在 115.6～817.8 ng/mL 与峰面积的 线性关系良好。R,R 型异构体平均回收率为 100.31%，RSD 值为 1.1%（n ＝9 ）。结论 建立的盐酸非那沙星 R,R 型异构体 HPLC 法拆分检查法方便、准确，能有效地控制盐酸非那沙星的质量。 关键词：盐酸非那沙星；R,R 型异构体；高效液相色谱 中图分类号：R927.2 文献标志码：A 文章编号：1674 - 5515(2015)07 - 0805 - 04 DOI: 10.7501/j.issn.1674-5515.2015.07.011 Determination of R,R isomer in finafloxacin hydrochloride active pharmaceutical ingredient by HPLC 1 2 1 WANG Dong , LI Xiao-bo , WANG Chen 1. Tianjin Key Laboratory of Cancer Prevention and Therapy, National Clinical Research Center for Cancer, Tianjin Medical University Cancer Institute and Hospital, Tianjin 300060, China 2. School of Pharmacy, Tianjin Medical University, Tianjin 300070, China Abstract: Objective To develop an HPLC method for determination of R,R isomer in finafloxacin hydrochloride active pharmaceutical ingredient. Methods The separation was performed on a Chiralpak AY-H column (250 mm × 4.6 mm, 5 μm) with n-heptane - isopropanol - diethylamine (75 ∶25 ∶0.1) as mobile phase. The flow rate was 1.0 mL/min with injection volume of 10 μL, the column temperature was 35 ℃, and the detection wavelength was set at 295 nm. Results Finafloxacin hydrochloride and R,R isomer had good linearity in the ranges of 101.2 — 813.1 ng/mL and 115.6 — 817.8 ng/mL. The average recovery of R,R isomer was 100.31% with RSD 1.1% (n=9). Conclusion The method is convenie