Method for measuring concentration of enantiomer of ibuprofen in chiral liquid-liquid extraction water phase by using high performance liquid chromatography (HPLC)

Abstract

A method for measuring the concentration of enantiomer of ibuprofen in a chiral liquid-liquid extracted water phase by using high performance liquid chromatography (HPLC) is a method for measuring the concentration of two types of enantiomer of ibuprofen in a water phase of a chiral liquid-liquid extraction system. The method comprises the following steps of: adding methanol-phosphate / phosphate buffered saline serving as a mobile phase by using an alpha 1- acid glycoprotein chiral column; and measuring the concentration of the two types of enantiomer of the ibuprofen in a water phase solution of the chiral liquid-liquid extraction system by using a calibration curve method under the condition of proper ultraviolet detection wavelength and proper ultraviolet detection flow velocity. By the method, base lines of the two types of enantiomer of the ibuprofen are separated from each other, and the concentration of the enantiomer of the ibuprofen can be accurately measured. The method is simple, quick, accurate and effective, is high in precision and reproducibility, and lays a foundation for setting an S-ibuprofen quality standard.

Description

technical field [0001] The invention relates to a method for measuring the concentration of ibuprofen enantiomers in the aqueous phase solution of a chiral liquid-liquid extraction system by using an HPLC method. Background technique [0002] Ibuprofen [(R,S)-2-(-4-isobutylphenyl)-propionic acid] is an important non-steroidal drug because of its analgesic, anti-inflammatory and antipyretic effects Far stronger than aspirin, phenylbutazone and paracetamol, it is favored by consumers and has occupied the top sales list of anti-inflammatory and analgesic drugs for many years. The α-position of the ibuprofen molecule is a chiral carbon atom, and there is a pair of optically active isomers. The chemical structural formula is: [0003] [0004] Modern pharmacological experiments have proved that its pharmacological activity is mainly produced by S-type ibuprofen, and the curative effect of S-type ibuprofen is about 160 times higher than that of R-type ibuprofen, and the main t...

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Problems solved by technology

[0005] So far, only a small number of documents have reported the chromatographic analysis methods of ibuprofen, mainly by the chiral mobile phase addition method and the direct analysis method of normal phase chromatography. The former is more representative by Li Chengping (Drug Analysis Journal, 2005,25(4):426-428) with Agilent Eclipse XDB-C 8 The column is used as an analytical column, with water:methanol:acetonitrile=78:17:5, the concentration of hydroxypropyl-β-cyclodextrin is 80mmol / L, 0.2% phosphoric acid, pH=4.50 mixed solution is used as the mobile phase, the flow rate 1.0ml / min, the resolution is about 1.42, and the retention times of the two enantiomers are 48min and 56min respectively. Although the separation effect of this method is acceptable, the analysis time is too long, and it often needs to be analyzed when performing liquid-liquid extraction experiments. There are many samples, this analysis method is not conducive to improving the efficiency of the experiment

Regarding the direct method of normal phase chromatography, researchers such as Crowther (Anal.Chem., 1984, 56, 2921-2926) attached a Pirkle-type chiral stationary phase to silica gel particles as a chiral filler. Alkane: Virahol=97: 3 (volume ratio) as mobile phase, realized the chromatographic resolution to ibuprofen racemate under the flow velocity of 2ml / min; Song Shaofang etc. (drug analysis impurity, 2002,22( 1):50-52) using Chiral OD-H column as the analytical column and n-hexane: acetic acid = 99:1 as the mobile phase, the enantiomers of ibuprofen were successfully separated. The separation of ibuprofen enantiomers, but the existing problem is that the chromatographic n-hexane as the mobile phase is expensive, and the analysis method is relatively harsh. The solution for dissolving the sample needs to be an organic solvent, and its polarity cannot be greater than that of the mobile phase Otherwise, the degree of separation will be reduced until the baseline separation cannot be achieved, which cannot meet the analysis requirements for the concentration of ibuprofen enantiomers in the aqueous phase of the chiral liquid-liquid extraction system

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