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Method for detecting 1, 3-dioxolane impurities

A dioxolane and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of low quantification limit and high sensitivity

Active Publication Date: 2020-08-28
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

[0004] There are no reported detection methods for impurity B and impurity C. Therefore, the development of detection methods for impurity B and impurity C is of great significance to the process development and quality control of related raw materials

Method used

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  • Method for detecting 1, 3-dioxolane impurities
  • Method for detecting 1, 3-dioxolane impurities
  • Method for detecting 1, 3-dioxolane impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Embodiment 1 detection method

[0061] Instrument conditions and reagents

[0062] Instruments: gas chromatograph, autosampler, Agilent GC\MS QQQ 7000D equipped with EI ion source, electronic analytical balance

[0063] Chromatographic column: capillary column with (5%-phenyl)-methyl polysiloxane stationary liquid (such as: Agilent HP-5MS, 30 m x 0.25 mm, 0.25 μm, or a column with equivalent performance)

[0064] Column temperature: the initial temperature is 80°C, keep it for 3 minutes, raise the temperature to 200°C at a rate of 15°C per minute, and keep it for 5 minutes;

[0065] Inlet temperature: 150°C Carrier gas: He

[0066] Split mode: Split carrier gas flow rate: 1mL / min

[0067] Split ratio: 10:1 GC run time: 16 min

[0068] Injection volume: 2µL

[0069] Mass Spectrometry Conditions:

[0070]

[0071] Reagents and reference substances

[0072] Dichloromethane: AR and above

[0073] Trans-4,5-dichloro-4,5-dimethyl-1,3-dioxolan-2-one (impurity B): pu...

Embodiment 2

[0094] Embodiment 2 System Applicability

[0095] The system suitability is realized by the S / N of impurity B and impurity C in the sensitivity solution and the RSD of the peak areas of impurity B and impurity C in the standard solution, and the S / N of impurity B and impurity C in the sensitivity solution is required All should not be less than 10; 6. The RSD of the peak areas of impurity B and impurity C in the standard solution should not be greater than 10.0%; in order to confirm the system suitability during the sequence operation, every 8 hours or sequence Finally, enter 1 reference solution, and the RSD of the peak areas of impurity B and impurity C in the reference solution for 6 consecutive reference solutions after the requirement should not exceed 10.0%; if it exceeds this range, an evaluation investigation should be carried out.

[0096] Solution preparation

[0097] Diluent: dichloromethane;

[0098] Blank solution: diluent;

[0099] According to the preparation...

Embodiment 3

[0103] Example 3 specificity

[0104] Specificity is achieved by determining whether the blank solution interferes with the detection of impurity B and impurity C, and the separation between impurity B and impurity C and adjacent peaks in the selective solution; the blank solution is required to have no interference to the detection, and the selective solution The separation between impurity B, impurity C and adjacent impurity peaks should not be less than 1.5.

[0105] Solution preparation

[0106] Diluent: dichloromethane;

[0107] Blank solution: diluent;

[0108] Impurity B stock solution: refer to Example 2 impurity B stock solution;

[0109] Impurity C stock solution: refer to Example 2 Impurity C stock solution;

[0110] Reference substance mixed stock solution: refer to the reference substance mixed stock solution under the item of Example 2;

[0111] Impurity B positioning solution: Accurately measure 1.0mL of impurity B stock solution, place it in a 100ml volume...

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Abstract

The invention provides a method for detecting 1, 3-butanediol in a sample by adopting a gas chromatography-mass spectrometry method. More especially, a gas chromatography-mass spectrometry method is adopted to detect trans-4, 5-dichloro-4, 5-dimethyl-1, 3-dioxolane-2-ketone and cis-4, 5-dichloro-4, 5-dimethyl-1, 3-dioxolane-2-ketone in a sample, wherein the sample is olmesartan medoxomil, azilsartan medoxomil, ampicillin and prulifloxacin, and chromatographic conditions adopted by adopting the detection method are as follows: a chromatographic column is a capillary column taking a (5%-phenyl)-methyl polysiloxane stationary liquid, and programmed heating is adopted; and the programmed heating is that the initial temperature of the column temperature is 80 DEG C, the temperature is kept for3 minutes, the temperature is increased to 200 DEG C at the speed of 15 DEG C per minute, and the temperature is kept for 5 minutes.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical analysis, in particular to a gas phase-mass spectrometry method for detecting the content of 1,3-dioxolane impurities in a sample, more specifically a gas phase-tandem mass spectrometry method for detecting trans- 4,5-dichloro-4,5-dimethyl-1,3-dioxolan-2-one and cis-4,5-dichloro-4,5-dimethyl-1,3 -Dioxolan-2-one. 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 cilexetil, lenamcillin, prulifloxacin, etc. can improve the bioavailability and stability of drugs. The preparation of DMDO-Cl in the prior art is generally prepared from 4,5-dimethyl-1,3-dioxol-2-one (DMDO) by chlorination with a chlorination reagent, and it is easy to produce trans-4,5-dichloro-4,5-dimethyl-1,3-dioxolan-2-one (impurity B, formula I) and cis-4,5-dichloro-4 ,5-Dimethyl-1,3-dioxol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/54
CPCG01N30/02G01N30/54
Inventor 张敏李达胜汤伟彬蔡强焦慎超
Owner 珠海润都制药股份有限公司
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