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Liquid chromatographic analysis method for detecting content of rearranged ester

A technology of liquid chromatography analysis and liquid chromatography, which is applied in the field of liquid chromatography analysis to detect the content of rearranged esters, can solve the problems of complex response factor gap of product impurities, unclear chromatographic conditions, etc., and achieve short analysis time, heavy Good performance and good peaking effect

Pending Publication Date: 2021-03-02
QINGDAO UNIV OF SCI & TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a fast, efficient and accurate analytical method for rearranged esters, to solve the problem of unclear chromatographic conditions caused by the use of liquid chromatography area normalization method for detecting rearranged ester content at present, and the actual production The complexity of the impurities in the product brings about a large technical problem in the response factors of the components in liquid chromatography.

Method used

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  • Liquid chromatographic analysis method for detecting content of rearranged ester
  • Liquid chromatographic analysis method for detecting content of rearranged ester
  • Liquid chromatographic analysis method for detecting content of rearranged ester

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Experimental program
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Effect test

Embodiment 1

[0059] 1.1 Reagents and instruments

[0060] Methanol: HPLC;

[0061] Rearranged ester standard sample: self-made purity 98.9%;

[0062] Analytical balance: 0.0001g;

[0063] Organic phase microporous membrane: 0.22μm;

[0064] Liquid chromatograph: U3000, Thermo Fisher, equipped with UV detector, equipped with

[0065] Autosampler;

[0066] Capillary column: C18 liquid chromatography column, 150mm×4.6mm×2.6μm, Thermo

[0067] flying company;

[0068] 1.2 Chromatographic method

[0069] a) Mobile phase: A: acetonitrile or methanol; B: 1% phosphoric acid or acetic acid aqueous solution

[0070] b) mobile phase ratio A:B=80:20;

[0071] c) Injection volume: 20.0 μL;

[0072] d) Column thermostat: 30°C;

[0073] e) Flow rate: 1mL / min;

[0074] f) Detection type: UV detector;

[0075] g) Detection wavelength: 222nm;

[0076] h) Chromatographic column: C18 liquid chromatography column, 150mm×4.6mm×2.6μm;

[0077] 1.3 Draw standard curve

[0078] Take the standard wor...

Embodiment 2

[0093] Embodiment 2 includes most of the technical features of Embodiment 1, and the difference with Embodiment 1 is that in Embodiment 2, the sampling position is the raw material of the production neutralization process, and about 70% of the material is rearranged ester, so the pre-treatment The method is as follows: take 1.0258g of the sample, put it into a 100mL volumetric flask, add mobile phase to constant volume and shake well as the sample stock solution, then remove 1mL of the sample stock solution, dilute it to volume with mobile phase in a 100mL volumetric flask, and use a 0.22μm filter membrane Analysis after filtration.

[0094] The present embodiment analyzes chromatogram such as Figure 4 According to this method, the content of rearranged esters is 69.511%.

[0095] Among them, in Figure 2-Figure 4 The vertical axis represents absorbance or absorbance, in Figure 2-Figure 4 Expressed in Absorbance.

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Abstract

The invention discloses a liquid chromatography analysis method of rearranged ester (II, alpha-methyl-4-(2-methyl propyl) phenylacetic acid-3-chloro-2, 2-dimethyl propyl ester), which comprises the steps of preparing an analysis sample, analyzing conditions of liquid chromatography, and carrying out qualitative and quantitative methods. The liquid chromatography conditions are as follows: a) a mobile phase: a first raw material is acetonitrile or methanol; the second raw material is 1% phosphoric acid or acetic acid aqueous solution; b) the ratio of the first raw material to the second raw material in the mobile phase is 80: 20; c) a sample injection volume is 20.0 [mu]L; d) a column oven temperature is 30 DEG C; e) a flow rate is 1 mL / min; f) a detection type is an ultraviolet detector; g) a detection wavelength is 222 nm; h) a chromatographic column is C18, 150 mm * 4.6 mm * 2.6 [mu]m, and a rearrangement ester residence time is 6.925 min. The quantitative method is an external standard method. The method disclosed by the invention is simple to operate and low in cost, and can be used for quickly, efficiently and accurately analyzing the rearranged ester.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a liquid chromatography analysis method for detecting the content of rearranged esters. Background technique [0002] Ibuprofen is an effective non-steroidal anti-inflammatory analgesic, and its production process is generally used in China at present. The aryl 1,2-transposition rearrangement method uses isobutylbenzene as a raw material, and is combined with 2- It can be prepared through the steps of Fuke acylation of chloropropionyl chloride, catalytic ketalization with neopentyl glycol, catalytic rearrangement, hydrolysis and acidification. The hydrolysis reaction of the process is that a certain concentration of rearranged esters reacts with sodium hydroxide to generate ibuprofen sodium salt and chlorohydrin, and the ibuprofen sodium salt is acidified to obtain ibuprofen, while the by-product chlorohydrin is alkali Etherification reaction can occur in a strong environment, ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/60G01N30/74
CPCG01N30/02G01N30/06G01N30/34G01N30/60G01N30/74G01N2030/047
Inventor 孔令启张玲周波杜德平隋明明夏丙堃于鹏寇祖星
Owner QINGDAO UNIV OF SCI & TECH
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