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Method for detecting 2, 2-dimethyl-1, 3-dichloropropane in ibuprofen

A technology of dichloropropane and a detection method is applied in the field of detecting 2,2-dimethyl-1,3-dichloropropane in ibuprofen, and can solve the problems of inability to correct hyperuricemia and the like

Active Publication Date: 2020-11-24
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

The treatment of gout is to relieve gout through anti-inflammation and analgesia, but it cannot correct hyperuricemia

Method used

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  • Method for detecting 2, 2-dimethyl-1, 3-dichloropropane in ibuprofen
  • Method for detecting 2, 2-dimethyl-1, 3-dichloropropane in ibuprofen
  • Method for detecting 2, 2-dimethyl-1, 3-dichloropropane in ibuprofen

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Experimental materials and instrument conditions

[0037] Experimental materials: acetonitrile, manufacturer: Merck & Co., Ltd.; 2,2-dimethyl-1,3-dichloropropane, manufacturer: TCI (Shanghai) Chemical Industry Development Co., Ltd.; ibuprofen , manufacturer: Hubei Encyclopedia Gelai Pharmaceutical Co., Ltd.; ultrapure water, manufacturer: Zhuhai Rundu Pharmaceutical Co., Ltd.

[0038] Instrument: Gas Chromatography Mass Spectrometry: 7890B&7000D GC / MS Triple Quad; Electronic Analytical Balance: GR-200, XSE205DU; Chromatographic Column: Agilent DB-624 30m×0.32mm, 1.8μm.

[0039]Determination method: inject the blank solution, sensitivity solution, reference solution and test solution into the liquid chromatograph respectively, and record the chromatogram. Siloxane; column temperature: the initial temperature is 40°C, keep for 5 minutes, raise the temperature to 100°C at a rate of 10°C per minute, then raise the temperature to 250°C at a rate of 50°C per minute, and ...

Embodiment 2

[0052] Embodiment 2 Detection method system applicability test of the present invention

[0053] System suitability is determined by measuring the peak signal-to-noise ratio of 2,2-dimethyl-1,3-dichloropropane in the sensitivity solution and 2,2-dimethyl-1,3-dichloropropane in the 5-pin reference solution. The RSD of the peak area is realized, and the signal-to-noise ratio of the 2,2-dimethyl-1,3-dichloropropane peak in the sensitivity solution should not be less than 3, and the 5-pin reference solution should be 2,2-dimethyl- The RSD of 1,3-dichloropropane peak area should not exceed 10.0%.

[0054] Prepare blank solution, sensitivity solution and reference 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, record the spectrogram, as figure 1 , figure 2 and image 3 , according to the formula conversion results are shown in the...

Embodiment 3

[0056] Embodiment 3 Detection method specificity test of the present invention

[0057] Specificity is determined by determining whether the blank solution interferes with the detection of 2,2-dimethyl-1,3-dichloropropane; Propane recovery is achieved. It is required that the blank solution should not interfere with the detection of 2,2-dimethyl-1,3-dichloropropane; before and after adding the sample, the recovery rate of 2,2-dimethyl-1,3-dichloropropane in the selective solution It should be between 80.0% and 120.0%.

[0058] Prepare the blank solution, 2,2-dimethyl-1,3-dichloropropane 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 spectrum, such as figure 1 , image 3 , Figure 4 and Figure 5 , and the specificity test results are shown in the fo...

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Abstract

The invention provides a method for detecting 2, 2-dimethyl-1, 3-dichloropropane in ibuprofen, an ibuprofen intermediate 3 can be subjected to side reaction in the hydrolysis process to possibly generate the 2, 2-dimethyl-1, 3-dichloropropane impurity, and the 2, 2-dimethyl-1, 3-dichloropropane impurity contains a genotoxic impurity warning group R-Cl, so that the content of the 2, 2-dimethyl-1,3-dichloropropane impurity can be detected according to the requirement of genotoxic impurities. According to the method, firstly, 6% cyanopropylphenyl-94% dimethyl polysiloxane or a chromatographic column with equivalent energy efficiency is used, and helium is used for applying pressure to the chromatographic column, so that the 2, 2-dimethyl-1, 3-dichloropropane in the ibuprofen is separated fromother substances, finally, the residual quantity of the 2, 2-dimethyl-1,3-dichloropropane in the ibuprofen can be determined, the detection sensitivity is greatly improved, the product quality is more effectively controlled, and higher quality requirements can be met

Description

technical field [0001] The invention belongs to the field of pharmaceutical analytical chemistry, and in particular relates to a method for detecting 2,2-dimethyl-1,3-dichloropropane in ibuprofen by a GC-MS method. Background technique [0002] Ibuprofen (CAS No.: 15687-27-1) is an antipyretic and analgesic non-steroidal anti-inflammatory drug. The English name is: Ibuprofen, and the Chinese name of its compound is: 4-isobutyl-α-methylbenzene acetic acid. The use of ibuprofen is that the drug metabolizes arachidene into mediator prostaglandins or other transmitters by inhibiting inducible inflammatory cyclooxygenase (COX2), thereby reducing the effects of prostaglandins (PGE1, PGE2, PGI2). Local tissue congestion, swelling, and heating. By inhibiting the activity of white blood cells and the release of lysosomes, it can reduce the pain sensitivity of local peripheral nerves to pain-causing substances such as bradykinin, reduce tissue impulses, and play an analgesic effect....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 李达胜汤伟彬王晴晴
Owner 珠海润都制药股份有限公司