（R）-丁酸缩水甘油酯中（S）-丁酸缩水甘油酯的液相色谱法测定
Liquid chromatographic estimation of (S) - glycidyl butyrate in (R) - glycidyl butyrate.
作者信息
Khan Mubeen Ahmad, Sinha Sukumar, Khandekar Nandkumar, Parashar Vikas
机构信息
Analytical Research Laboratory, Glenmark Research Center, Glenmark Generics Limited Navi Mumbai, Maharashtra, India.
出版信息
J Nat Sci Biol Med. 2011 Jul;2(2):180-4. doi: 10.4103/0976-9668.92331.
AIM
The present study was undertaken out of a commercial need for the synthesis of Linezolid with impurity limits within the specification.
MATERIALS AND METHODS
(R)-Glycidyl butyrate (RGB) is raw material for the synthesis of Linezolid drug substance. This RGB contains (S)-(+)-Glycidyl butyrate (SGB) and SGB appears in same concentration in the final Active Pharmaceutical Ingredient. So, a normal phase high-performance liquid chromatography (HPLC) method has been developed to determine the SGB level in the raw material. RGB and SGB were separated using an HPLC system equipped with quaternary gradient pumps on a Daicel chiralpak AD-H (250 × 4.6 mm) column with a mobile phase consisting 2.0 ml of ethanol in 1 000 ml of n-hexane. A 0.5 ml/minute flow rate and a 10 μl injection volume was used and the compounds were detected at 215 nm.
RESULTS
Method validation parameters demonstrated the same to be reliable, reproducible, and accurate one.
CONCLUSION
Thus, the present study may be used for regular quality control of RGB to improve commercial feasibility for the synthesis of Linezolid.
目的
本研究是出于商业需求而开展的，旨在合成杂质限度符合规格的利奈唑胺。
材料与方法
（R）-丁酸缩水甘油酯（RGB）是合成利奈唑胺原料药的原料。该RGB含有（S）-（+）-丁酸缩水甘油酯（SGB），且SGB在最终活性药物成分中的浓度相同。因此，已开发出一种正相高效液相色谱（HPLC）法来测定原料中的SGB水平。使用配备四元梯度泵的HPLC系统，在大赛璐手性pak AD-H（250×4.6 mm）色谱柱上分离RGB和SGB，流动相为1000 ml正己烷中含2.0 ml乙醇。流速为0.5 ml/分钟，进样体积为10 μl，在215 nm处检测化合物。
结果
方法验证参数表明该方法可靠、可重现且准确。
结论
因此，本研究可用于RGB的常规质量控制，以提高利奈唑胺合成的商业可行性。
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