摘要
目的 以万古霉素为手性选择子 ,建立酮洛芬对映体以手性柱法和流动相添加剂法进行手性分析的方法。方法 考察万古霉素用量、有机改性剂用量及缓冲液pH值对酮洛芬对映体手性拆分的影响 ,并进行了定量分析的方法验证。结果 两种拆分方法都使酮洛芬对映体达到了基线分离 ,都适合于酮洛芬对映体的定性和定量分析。结论 所建立的两种方法均可用于S (+) 酮洛芬的光学纯度检测。
Aim To establish HPLC chiral separation method for ketoprofen enantiomers by using Chirobiotic V chiral seperation phase(CSP) (A) and vancomycin as chiral mobile phase additives (B). Methods The separation was first performed on Chirobiotic V CSP with the mobile phase of terahydrofran(THF) 0 5% triethylanine acetate(TEAA) buffer (15∶85) at the flow rate of 0 7 mL·min -1 . When using vancomycin as chiral mobile phase additive, the separation was carried out on C 8 column (150 mm×4 6 mm), the mobile phase was methanol 0 25% TEAA buffer (50∶50), the flow rate was 0 7 mL·min -1 . The effects of the concentration of vancomycin, organic modifier and the pH of the buffer on the resolution of ketoprofen enantiomers were investigated. Also, the feasibility of these two methods to be used as quantitative method was studied. Results Ketoprofen enantiomers were separated at a baseline level under the chromatographic condition of both methods A and B, the resolution was 2 28 and 2 22, respectively. In method A the linearity of enantiomer was obtained from 0 5 mg·L -1 to 100 mg·L -1 , the detection limit was 1 μg·L -1 . When using vancomycin as mobile phase additive the system was shown to have a high efficiency. In this system, the assay of enantiomer is linear from 2 5 mg·L -1 to 250 mg·L -1 . The detection limit was 14 5 μg·L -1 . Conclusion Both methods can be used to detect optical purity of S (+) ketoprofen.
出处
《药学学报》
CAS
CSCD
北大核心
2003年第3期211-214,共4页
Acta Pharmaceutica Sinica
关键词
高效液相色谱
手性柱
手性流动相添加剂
酮洛芬
对映体
万古霉素
high performance liquid chromatography
chiral stationary phase
chiral mobile phase additive
ketoprofen
enantiomer
vancomycin
