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采用手性AGP柱对酮咯酸进行对映体选择性分析的新型手性反相高效液相色谱法。

New chiral reverse phase HPLC method for enantioselective analysis of ketorolac using chiral AGP column.

作者信息

Dubey Sunil K, Hemanth Jangala, Venkatesh K Chiranjeevi, Saha R N, Pasha S

机构信息

Department of Pharmacy, Birla Institute of Technology & Science, Pilani, India.

Institute of Genomics and Integrative Biology, Mall Road, Delhi, India.

出版信息

J Pharm Anal. 2012 Dec;2(6):462-465. doi: 10.1016/j.jpha.2012.07.006. Epub 2012 Jul 22.

DOI:10.1016/j.jpha.2012.07.006
PMID:29403784
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC5760942/
Abstract

A simple, specific, precise, sensitive and rapid reverse phase-HPLC method was developed for determination of ketorolac enantiomers, a potent nonnarcotic analgesic in pharmaceutical formulations. The method was developed on a chiral AGP column. Mobile phase was 0.1 M sodium phosphate buffer (pH 4.5): Isopropanol (98:2, v/v), at a flow rate of 1 mL/min with run time of 15 min. Ultraviolet detection was made at 322 nm. The linearity range was 0.02-10 μg/mL for each of the enantiomers. The mobile phase composition was systematically studied to find the optimum chromatographic conditions. Validation of the method under the conditions selected showed that it was selective and precise and that the detector response was linear function of ketorolac.

摘要

开发了一种简单、特异、精确、灵敏且快速的反相高效液相色谱法,用于测定酮咯酸对映体,酮咯酸是药物制剂中一种有效的非麻醉性镇痛药。该方法采用手性AGP柱。流动相为0.1M磷酸钠缓冲液(pH 4.5):异丙醇(98:2,v/v),流速为1mL/min,运行时间为15分钟。在322nm处进行紫外检测。每种对映体的线性范围为0.02 - 10μg/mL。系统研究了流动相组成以找到最佳色谱条件。在所选择的条件下对该方法进行验证表明,它具有选择性和精确性,并且检测器响应是酮咯酸的线性函数。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/0aaf/5760942/cd2fed477a81/fx00.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/0aaf/5760942/25cfd6a83500/gr1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/0aaf/5760942/c3903c1e3d5e/gr2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/0aaf/5760942/cd2fed477a81/fx00.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/0aaf/5760942/cd2fed477a81/fx00.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/0aaf/5760942/25cfd6a83500/gr1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/0aaf/5760942/c3903c1e3d5e/gr2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/0aaf/5760942/cd2fed477a81/fx00.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/0aaf/5760942/cd2fed477a81/fx00.jpg

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本文引用的文献

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Two-dimensional liquid chromatography-ion trap mass spectrometry for the simultaneous determination of ketorolac enantiomers and paracetamol in human plasma: application to a pharmacokinetic study.二维液相色谱-离子阱质谱法同时测定人血浆中酮咯酸对映体和对乙酰氨基酚:在药代动力学研究中的应用
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Optical resolution of a series of potential cholecystokinin antagonist 4(3H)-quinazolone derivatives by chiral liquid chromatography on alpha1-acid glycoprotein stationary phase.在手性α1-酸性糖蛋白固定相上通过手性液相色谱法对一系列潜在的胆囊收缩素拮抗剂4(3H)-喹唑啉酮衍生物进行光学拆分。
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An indirect (derivatization) and a direct HPLC method for the determination of the enantiomers of ketorolac in plasma.一种间接(衍生化)和直接高效液相色谱法用于测定血浆中酮咯酸对映体。
J Pharm Biomed Anal. 1996 Dec;15(3):403-17. doi: 10.1016/s0731-7085(96)01856-0.
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The problem of racemization in the stereospecific assay and pharmacokinetic evaluation of ketorolac in human and rats.酮咯酸在人和大鼠体内的立体特异性分析及药代动力学评估中的消旋化问题。
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Stereoselective analysis of ketorolac in human plasma by high-performance liquid chromatography.高效液相色谱法对人血浆中酮咯酸的立体选择性分析。
Chirality. 1993;5(1):31-5. doi: 10.1002/chir.530050107.
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Determination of ketorolac enantiomers in plasma using enantioselective liquid chromatography on an alpha 1-acid glycoprotein chiral stationary phase and ultraviolet detection.使用α1-酸性糖蛋白手性固定相和紫外检测的对映体选择性液相色谱法测定血浆中的酮咯酸对映体。
J Chromatogr B Biomed Appl. 1994 Aug 5;658(1):177-82. doi: 10.1016/0378-4347(94)00228-2.
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J Chromatogr B Biomed Appl. 1994 Nov 4;661(1):165-7. doi: 10.1016/0378-4347(94)00333-5.
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