Method for detecting 4-chloro-4-methyl-5-methylene-1, 3-dioxolane-2-ketone

A detection method and a technique for dioxolane, applied in the field of gas phase-tandem mass spectrometry

Pending Publication Date: 2021-06-08
珠海润都制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] No detection method for impurity A has been reported. Therefore, the development of a detection method for impurity A is of great significance to the process development and quality control of related raw materials

Method used

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  • Method for detecting 4-chloro-4-methyl-5-methylene-1, 3-dioxolane-2-ketone
  • Method for detecting 4-chloro-4-methyl-5-methylene-1, 3-dioxolane-2-ketone
  • Method for detecting 4-chloro-4-methyl-5-methylene-1, 3-dioxolane-2-ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Embodiment 1 detection method

[0069] Instrument conditions and reagents

[0070] Instruments: gas chromatograph, autosampler, Agilent GC\MS QQQ 7000D equipped with EI ion source, electronic analytical balance

[0071] Chromatographic column: capillary column with (14%-cyanopropyl-phenyl)-methyl polysiloxane as the stationary liquid (such as: AgilentDB-1701, 30 m x 0.25 mm, 1 μm or a column with equivalent performance)

[0072] Column temperature: the initial temperature is 150°C, keep for 1 minute; raise the temperature to 200°C at a rate of 35°C per minute, keep for 5 minutes; raise the temperature to 250°C at a rate of 30°C per minute, and keep for 3 minutes.

[0073] Injection port temperature: 130°C Carrier gas: He

[0074] Split mode: split Carrier gas flow: 1mL / min

[0075] Split ratio: 10:1 GC run time: 12.095min

[0076] Injection volume: 1µL

[0077] Mass Spectrometry Conditions:

[0078]

[0079] Reagents and reference substances

[0080] Chlorofor...

Embodiment 2

[0100] Embodiment 2 System Applicability

[0101]System suitability is determined by the S / N of 4-chloro-4-methyl-5-methylene-1,3-dioxolane-2-one in the sensitivity solution and 6 against 4-chloro- 4-methyl-5-methylene-1,3-dioxolane-2-one peak area is achieved by RSD, requiring sensitivity solution 4-chloro-4-methyl-5-methylene- The S / N of 1,3-dioxolane-2-one should not be less than 3,6 for 4-chloro-4-methyl-5-methylene-1,3-dioxolane in the reference solution The RSD of the -2-ketone peak area should not be greater than 10.0%. In order to confirm the system suitability during the sequence operation, inject a freshly prepared reference solution every 8 hours or at the end of the sequence during the verification process. The RSD of the peak area per unit concentration of 4-chloro-4-methyl-5-methylene-1,3-dioxolan-2-one in the reference solution for 6 consecutive points should not be greater than 10.0%; if it exceeds this range, An evaluation survey should be done.

[0102] Th...

Embodiment 3

[0106] Example 3 specificity

[0107] Specificity is determined by determining whether the blank solution interferes with the detection of 4-chloro-4-methyl-5-methylene-1,3-dioxolane-2-one, and 4-chloro-4- The separation between methyl-5-methylene-1,3-dioxolan-2-one and adjacent peaks is achieved; the blank solution is required to have no interference with the detection, and 4-chloro-4-in the selective solution The separation between methyl-5-methylene-1,3-dioxolane-2-one and adjacent impurity peaks should not be less than 1.5, and 4-chloro-4-methyl-5- The recovery rate of methylene-1,3-dioxolan-2-one should be between 80.0% and 120.0%.

[0108] The solution was prepared, and samples were injected according to the conditions of Example 1. The test results are shown in Table 9 and Table 10.

[0109]

[0110]

[0111] Wherein, need testing product brings into peak area=need testing product solution peak area ÷ need testing product solution sampling volume * selective sol...

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Abstract

The invention provides a method for detecting the impurity content of 4-chloro-4-methyl-5-methylene-1, 3-dioxolane-2-ketone in a sample by adopting a gas chromatography-mass spectrometry method, the sample is olmesartan medoxomil, azilsartan, azilsartan medoxomil, azilsartan medoxomil potassium, lenampicillin and prulifloxacin, the sample does not need to be specially treated, and no matrix influence exists. Chromatographic conditions adopted by the detection method are as follows: a chromatographic column is a capillary column taking (14%-cyanopropyl-phenyl)-methylpolysiloxane as a stationary liquid, and temperature programming is adopted; the temperature programming is as follows: the initial column temperature is 150 DEG C, and the temperature is kept for 1 minute; the temperature raises to 200 DEG C at the speed of 35 DEG C per minute, and the temperature is kept for 5 minutes; and the temperature raises to 250 DEG C at the speed of 30 DEG C per minute, and the temperature is kept for 3 minutes.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical analysis, and in particular relates to a method for detecting the impurity content of 4-chloro-4-methyl-5-methylene-1,3-dioxolane-2-one in a sample by using a gas phase-mass spectrometry method, More specifically, the gas phase-tandem mass spectrometry method is used to detect the impurity content of 4-chloro-4-methyl-5-methylene-1,3-dioxolane-2-one in the sample. Background technique [0002] 4-Chloromethyl-5-methyl-1,3-dioxol-2-one (DMDO-Cl) is an important chemical intermediate, which can be used to synthesize olmesartan medoxomil, azil Sartan, azilsartan medoxomil, azilsartan medoxomil potassium, lenamcillin, prulifloxacin, etc., can improve the bioavailability and stability of drugs. Literature (SHOJI IKEDA, YASUSHI TAKEBE, RYOICHIHIRAYAMA, FUMIO SAKAMOTO, KOJI IUCHI, GORO TSUKAMOTO. A Convenient and Practical Preparation of 4-Chloromethyl-5-methyl-1, 3-dioxol-2-one[J]. Chemical and P...

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 蔡强汤伟彬张敏李达胜
Owner 珠海润都制药股份有限公司
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