Method for detecting ibuprofen raw material impurity F

Abstract

The invention belongs to the field of medicine quality detection and in particular relates to a method for detecting an ibuprofen raw material impurity F. By adopting the method provided by the invention, the ibuprofen raw material impurity F can be effectively detected, the method is good in specificity and good in durability, the flowing velocity, the column temperature, the wavelength and the flow phase ratio can be changed, and the ibuprofen raw material impurity F can be accurately quantitatively detected. Compared with a conventional pharmacopeia method, the method is capable of simply,rapidly and conveniently detecting the ibuprofen raw material impurity F.

Description

technical field [0001] The invention belongs to the field of drug quality detection, in particular to a method for detecting the impurity F of ibuprofen raw materials. Background technique [0002] Ibuprofen is the only antipyretic drug for children jointly recommended by the World Health Organization and the US FDA. The impurity F is an isomeric impurity in ibuprofen. The major pharmacopoeias such as JP, ChP, USP, BP, and EP are consulted, and the impurity F is all controlled, but the detection methods are different. [0003] JP is the same as the Chinese Pharmacopoeia, and both use the TCL method to detect impurity F, which is cumbersome to operate, cannot be accurately quantified, and has low sensitivity. [0004] USP uses impurity F as another unknown impurity for liquid chromatography control. This method is more sensitive than thin-layer chromatography, but the specificity is not strong enough. [0005] The BP method is the same as that of EP8.0, both of which use de...

AI Technical Summary

Problems solved by technology

During the verification of the method, it was found that the sensitivity of the method could not meet the requirements, the repeatability was poor, and the baseline fluctuated greatly, and the verification results could not meet the measurement requirements.

The reasons are analyzed as follows: ①This method needs to methylate the sample first, the derivatization operation is relatively complicated, the parallelism of the test is not easy to control, and the methylation reagent is likely to have a certain impact on the baseline of the sample determination; ②In the gas chromatography Under the conditions, the concentration of the sample is too high, and the non-split mode is used. During the experiment, the instrument system is easily contaminated, and the baseline fluctuates greatly.

③ The sensitivity of impurity F is too small, and it is easily affected by baseline fluctuations, resulting in unsatisfactory verification results

[0006] In addition, a detection literature about impurity F was found "HPLC determination of impurity F in ibuprofen injection", this method also adopts normal phase chromatography, and the literature mobile phase is n-hexane-ethyl acetate-trifluoroacetic acid ( 95:5:0.5), and its existing problems are: ① trifluoroacetic acid has irritating odor and toxicity, which is not conducive to the safe operation of experimenters;

③Using the method in the literature, the number of theoretical plates of the impurity F is small, and the separation degree is not high

Images