Ye Xiao-xia, Yu Xiong
Shanghai Institute of Pharmaceutical Industry, Shanghai 200040, China.
Yao Xue Xue Bao. 2003 Mar;38(3):211-4.
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).
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 C8 column (150 mm x 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.
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 detectionlimit was 1 microgram.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 micrograms.L-1.
Both methods can be used to detect optical purity of S-(+)-ketoprofen.
采用手性冠醚V手性分离固定相（CSP）（A）和万古霉素作为手性流动相添加剂（B）建立酮洛芬对映体的高效液相色谱手性分离方法。
首先在Chirobiotic V CSP上进行分离，流动相为四氢呋喃（THF）-0.5%三乙胺乙酸盐（TEAA）缓冲液（15:85），流速为0.7 mL·min-1。当使用万古霉素作为手性流动相添加剂时，在C8柱（150 mm×4.6 mm）上进行分离，流动相为甲醇-0.25%TEAA缓冲液（50:50），流速为0.7 mL·min-1。考察了万古霉素浓度、有机改性剂和缓冲液pH对酮洛芬对映体分离度的影响。同时，研究了这两种方法作为定量方法的可行性。
在方法A和方法B的色谱条件下，酮洛芬对映体均能达到基线分离，分离度分别为2.28和2.22。在方法A中，对映体的线性范围为0.5 mg·L-1至100 mg·L-1，检测限为1 μg·L-1。当使用万古霉素作为流动相添加剂时，该系统显示出高效性。在该系统中，对映体的测定线性范围为2.5 mg·L-1至250 mg·L-1，检测限为14.5 μg·L-1。
两种方法均可用于检测S-(+)-酮洛芬的光学纯度。
