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A kind of detection method of 3-chloro-2,2-dimethyl-1-propanol in ibuprofen

A detection method and dimethyl technology, applied in the field of pharmaceutical analysis, can solve problems such as inability to control product quality and quality requirements more effectively, unclear chromatographic column conditions, and deviation in detection results, achieving low cost and strong specificity. , the effect of high accuracy

Active Publication Date: 2022-04-08
珠海润都制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production process commonly used in China for ibuprofen is the aryl 1,2-transposition rearrangement method. This method uses isobutylbenzene as a raw material, and undergoes acylation with 2-chloropropionyl chloride and neopentyl glycol. It is prepared by catalytic ketalization, catalytic rearrangement, hydrolysis, acidification and other steps. During the production process, the impurity 3-chloro-2,2-dimethyl-1-propanol will be generated. The magazine is detected at this stage The method is mainly the gas chromatographic area normalization method, the chromatographic column conditions are not clear, the product impurities in actual production are more complex, and the response factors of each component in the gas chromatogram have a large gap, so simply use the area normalization method Unable to accurately determine the content of 3-chloro-2,2-dimethyl-1-propanol
[0003] Patent CN111272900A records the use of gas chromatography to detect the content of 3-chloro-2,2-dimethyl-1-propanol. The chromatographic column used is a quartz capillary chromatographic column, and its specification is TG-wax30m×0.25mm× 0.25μm, the solvent used is methanol, the detection method provided in the patent has the disadvantages of time-consuming, deviation of the detection results, etc., and the detection sensitivity is poor, and the product quality cannot be controlled more effectively and can meet higher quality requirements

Method used

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  • A kind of detection method of 3-chloro-2,2-dimethyl-1-propanol in ibuprofen
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  • A kind of detection method of 3-chloro-2,2-dimethyl-1-propanol in ibuprofen

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Effect test

Embodiment 1

[0035] (1) Experimental materials and instrument conditions

[0036] Experimental materials: acetonitrile, manufacturer: Merck KGaA; ibuprofen, manufacturer: Hubei Baikelai Pharmaceutical Co., Ltd.; 3-chloro-2,2-dimethyl-1-propanol, manufacturer: Tokyo Chemical Industry Co., Ltd.; ultrapure water, manufacturer: Zhuhai Rundu Pharmaceutical Co., Ltd.

[0037] Instrument: Gas Chromatography Mass Spectrometry: 7890B&7000D GC / MS Triple Quad; Electronic Analytical Balance: XSE205DU, GR-200; Chromatographic Column: Agilent HP-5MS 30m×0.25mm, 0.25μm.

[0038] Inject the blank solution, reference solution, sensitivity solution and test solution into the gas chromatograph respectively, record the chromatogram, and the chromatographic conditions are as follows: chromatographic column: use (5% phenyl)-methylpolysiloxane as filler; column temperature : The initial temperature is 40°C, keep it for 5 minutes, raise the temperature to 100°C at a rate of 10°C per minute, then raise the temper...

Embodiment 2

[0051] Embodiment 2 Detection method system applicability test of the present invention

[0052] System suitability is determined by measuring the peak signal-to-noise ratio of 3-chloro-2,2-dimethyl-1-propanol in the sensitivity solution, 3-chloro-2,2-dimethyl-1-propanol in the 5-pin reference solution The RSD of the peak area of ​​propanol is realized, and the signal-to-noise ratio of the 3-chloro-2,2-dimethyl-1-propanol peak in the sensitivity solution should not be less than 3, and the 5-pin reference solution should be 3-chloro-2 , 2-dimethyl-1-propanol peak area meter RSD should not be greater than 10.0%.

[0053] Prepare blank solution, reference solution and sensitivity solution as described in Example 1, under the chromatographic conditions described in Example 1, enter 1 needle of blank solution, 1 needle of sensitivity solution, 5 needles of reference solution, obtain the chromatogram, as figure 1 , figure 2 with image 3 , according to the formula conversion res...

Embodiment 3

[0055] Embodiment 3 Detection method specificity test of the present invention

[0056] Specificity is determined by determining whether the blank solution interferes with the detection of 3-chloro-2,2-dimethyl-1-propanol; before and after sample addition, the selective solution of 3-chloro-2,2-dimethyl-1 -Propanol recovery achieved. It is required that the blank solution should not interfere with the detection of 3-chloro-2,2-dimethyl-1-propanol; The recovery rate should be between 80.0% and 120.0%.

[0057] Prepare the blank solution, 3-chloro-2,2-dimethyl-1-propanol stock solution, reference solution, test solution, and selective solution as described in Example 1. After the system is balanced, inject 1 needle of the blank solution , 3 needles of reference solution, 1 needle of test solution, 3 needles of selective solution, record the chromatogram, such as figure 1 , image 3 , Figure 4 with Figure 5 , and the specificity test results are as follows:

[0058]

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Abstract

The invention provides a method for detecting 3-chloro-2,2-dimethyl-1-propanol in ibuprofen, 3-chloro-2,2-dimethyl-1-propanol contains a warning structure Toxic substances, there may be incomplete reaction in the reaction process, but remain in the ibuprofen bulk drug, in order to detect the content of 3-chloro-2,2-dimethyl-1-propanol in ibuprofen, this paper The invention proposes a gas chromatography-mass spectrometry detection method for 3-chloro-2,2-dimethyl-1-propanol in ibuprofen. The degree, limit of quantification, limit of detection and durability are in full compliance with the guidelines for method validation in ICH Q2 and the four 9101 guidelines of the Chinese Pharmacopoeia, and can be used for the quality control of ibuprofen APIs.

Description

technical field [0001] The invention relates to the technical field of medical analysis, in particular to a method for detecting 3-chloro-2,2-dimethyl-1-propanol in ibuprofen. Background technique [0002] Ibuprofen is an antipyretic and analgesic non-steroidal anti-inflammatory drug. It is a kind of anti-inflammatory drug that does not contain a steroidal structure. It has the functions of reducing fever and relieving the discomfort caused by pain, but it has no effect on those with normal body temperature, and will not lower their body temperature; ibuprofen and naproxen belong to the aryl propionic acid antipyretic and analgesic It has obvious anti-inflammatory, antipyretic, and analgesic effects, and its strength is equivalent to that of aspirin. It has a certain inhibitory effect on platelet function and can prolong the bleeding time. At present, the production process commonly used in China for ibuprofen is the aryl 1,2-transposition rearrangement method. This method ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/72
CPCG01N30/02G01N30/72
Inventor 李达胜汤伟彬蔡强王晴晴
Owner 珠海润都制药股份有限公司