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Liquid chromatographic analysis method for detecting content of 1-chloroethyl-4-isobutylbenzophenone

A technology of liquid chromatography analysis and ketone, which is applied in the field of liquid chromatography analysis to detect the content of ketone, can solve the problems that the content of ketone cannot be reasonably judged, the expression formula cannot be obtained, etc., and the analysis time is short, the accuracy is high, good reproducibility

Pending Publication Date: 2022-02-11
SHANDONG XINHUA PHARMA CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to provide a fast, efficient and accurate analytical method for ketone, which is used to solve the problem of obtaining the expression formula of the standard curve that cannot be obtained when the liquid chromatography analysis method is used to detect the content of ketone at present, resulting in unreasonable The technical problem of judging the content of chlorketone corresponding to each concentration range

Method used

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  • Liquid chromatographic analysis method for detecting content of 1-chloroethyl-4-isobutylbenzophenone
  • Liquid chromatographic analysis method for detecting content of 1-chloroethyl-4-isobutylbenzophenone
  • Liquid chromatographic analysis method for detecting content of 1-chloroethyl-4-isobutylbenzophenone

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Experimental program
Comparison scheme
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Embodiment 1

[0066] 1.1 Reagents and instruments

[0067] Methanol: HPLC;

[0068] Chlorone standard sample: self-made purity 99.2%;

[0069] Analytical balance: 0.0001g;

[0070] Organic phase microporous membrane: 0.22μm;

[0071] Liquid chromatograph: U3000, Thermo Fisher, equipped with UV detector, equipped with automatic sampler;

[0072] Capillary column: C18 liquid chromatography column, 250mm×4.6mm×2.6μm, Thermo Fisher;

[0073] 1.2 Chromatographic method

[0074] a) Mobile phase: A: acetonitrile or methanol; B: 1% phosphoric acid or acetic acid aqueous solution

[0075] b) mobile phase ratio A:B=80:20;

[0076] c) Injection volume: 20.0 μL;

[0077] d) Column thermostat: 30°C;

[0078] e) Flow rate: 1mL / min;

[0079] f) Detection type: UV detector;

[0080] g) Detection wavelength: 222nm;

[0081] h) Chromatographic column: C18 liquid chromatography column, 250mm×4.6mm×2.6μm;

[0082] 1.3 Draw standard curve

[0083] Take the standard working solution respectively, an...

Embodiment 2

[0098] 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 for the production of the condensation process, and about 50% of the material is ketone, so the pretreatment method is as follows : Take 5.0258g of sample, put it into a 100mL volumetric flask, add mobile phase to constant volume and shake well as the sample stock solution, then take 1mL of sample stock solution, dilute it to constant volume with mobile phase in a 100mL volumetric flask, and filter it with a 0.22μm filter membrane Injection analysis.

[0099] The present embodiment analyzes chromatogram such as Figure 4 According to this method, the content of ketone is calculated to be 47.211%.

[0100] Among them, in Figure 2-Figure 4 The vertical axis of represents absorbance or absorbance, in Figure 2-Figure 4 Expressed in Absorbance.

[0101] It can be seen that the present invention is ...

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Abstract

The invention discloses a liquid chromatographic analysis method of 1-chloroethyl-4-isobutylbenzophenone. The method comprises the following steps of: S1, preparing a sample solution to be detected; S2, carrying out chromatographic detection on the sample solution to be detected; S3, preparing a standard solution with the equal difference being a first concentration gradient A; S4, drawing a first standard curve; S5, optimally preparing a standard solution with the equal difference being a second concentration gradient B; S6, optimizing the first standard curve into a second standard curve; S7, calculating an expression formula of the second standard curve; and S8, obtaining the content of 1-chloroethyl-4-isobutylbenzophenone in the sample to be detected. According to the method disclosed by the invention, the curve for acquiring the curvature peak value position of the drawn standard curve is optimized for detecting the content of 1-chloroethyl-4-isobutylbenzophenone, and then the accurate expression formula is acquired based on the optimized curve, so that the expression formula corresponding to the curve-shaped standard curve can be acquired; the 1-chloroethyl-4-isobutylbenzophenone content at the corresponding concentration value position of the sample to be detected is solved based on the expression formula; and whether the impurities of similar products meet the standard or not can be quickly judged.

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 ketone. 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. In the ketalization process of this process, chlorone and neopentyl glycol are used as raw materials, dilute sulfuric acid is used as a catalyst, and petroleum ether is used as a solvent. The ketalization reaction is internationally recognized as the core control step for the production of ibuprofen. Ketone (1-chloroethyl-4-isobutylbenzophenone) is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/74G01N30/8675G01N2030/047
Inventor 杜德平周波岳金彩徐文辉寇祖星夏丙堃贾建波于鹏孙科
Owner SHANDONG XINHUA PHARMA CO LTD
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