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Method for detecting related impurities of dipropylmalonic acid

A kind of technology of dipropylmalonic acid and dipropylmalonic acid monoethyl ester, which is applied in the detection field of dipropylmalonic acid-related impurities

Active Publication Date: 2021-06-04
SICHUAN CREDIT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the process evaluation and quality control problems of sodium valproate intermediat

Method used

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  • Method for detecting related impurities of dipropylmalonic acid
  • Method for detecting related impurities of dipropylmalonic acid
  • Method for detecting related impurities of dipropylmalonic acid

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0056] Example 1

[0057] Chromatographic conditions:

[0058] Column: InfinityLab Poroshell 120SB-AQ (4.6 × 150mm, 2.7μm)

[0059] Mobile phase: mobile phase A: 0.02mol / l Nah 2 PO 4 Solution, pH value of phosphoric acid to 2.0;

[0060] Mobile phase B: acetonitrile

[0061] Hand elution conditions:

[0062]

[0063] Flow speed: 0.8ml / min

[0064] Test wavelength: 205 nm

[0065] Number of injections: 5μL

[0066] Solution: Take the amount of dipropylpropylene acid reaction, 10 ml of volumetric flask, dissolved with a diluent (water-acetonitrile 50:50) to prepare a solution containing 10 to 30 mg of a solution of 10 to 30 mg per 1 ml, as a test Solution.

[0067] Measurement method: According to the above chromatographic conditions, take a blank solution, and the test solution is sampled separately, record the chromatogram, and the chromatogram of the test solution. figure 1 Among them, the retention time of diopropylpropanic acid (a) is 8.710 min, and the retention time of ...

Example Embodiment

[0068] Example 2

[0069] Chromatographic conditions:

[0070] Column: InfinityLab Poroshell 120SB-AQ (4.6 × 150mm, 2.7μm)

[0071] Mobile phase: mobile phase A: 0.02mol / l Nah 2 PO 4 Solution, pH value of phosphoric acid to 2.0;

[0072] Mobile phase B: acetonitrile

[0073] Hand elution conditions:

[0074]

[0075] Flow speed: 0.8ml / min

[0076] Test wavelength: 205 nm

[0077] Number of injections: 5μL

[0078] Diluent: Mobile phase A- Mobile phase B (50:50)

[0079] Solution formulation: 10 mg of compound B, C, D, E, F and G, precisely weighted, respectively, in 10ml volumetric flask, dissolved with diluents and dilute to the scale, shake, as impurities B, C , D, E, F, G Tsi; Ideal of about 1.0 g of dipropylpropylene, 50 ml of volumetric flask, and then add 1.0 ml of each impurity control stock solution, dissolved with a diluent and diluted to The scale, shake, as a test solution (each impurity content is about 0.1%, respectively).

[0080] Measurement: According to the ...

Example Embodiment

[0081] Example 3

[0082] Chromatographic conditions:

[0083] Column: InfinityLab Poroshell 120SB-AQ (4.6 × 150mm, 2.7μm)

[0084] Mobile phase: mobile phase A: 0.02mol / l Nah 2 PO 4 Solution, pH value of phosphoric acid to 2.0;

[0085] Mobile phase B: acetonitrile

[0086] Hand elution conditions:

[0087]

[0088] Flow speed: 0.8ml / min

[0089] Test wavelength: 205 nm

[0090] Number of injections: 5μL

[0091] Diluent: Mobile phase A- Mobile phase B (50:50)

[0092] The test solution is prepared: 10 mg of compound B, C, D, E, F and G, precisely weighted, respectively, in 10 ml of volumetric flask, dissolved with diluents and dilute to the scale, shake well, as impurities B, C, D, E, F, G Tsi; weigh 1.0 g of dipropylpropylene acid, set 50 ml of volumetric flask, and then add 1.0 ml of each impurity control stock solution, and dissolve with a diluent. And diluted to the scale, shake well, as a test solution (each impurity content is about 0.1%, respectively).

[0093] Meas...

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Abstract

The invention provides a method for detecting dipropylmalonic acid (a sodium valproate synthetic intermediate) and related impurities thereof. The method can also be used for detecting dipropylmalonic acid (A) in sodium valproate. The method adopts a high performance liquid chromatograph (HPLC) for determination, and comprises the following specific operation steps: (1) taking a sample to be detected, and preparing a test sample solution; and (2) taking the test solution, and detecting by using an instrument. The method can effectively separate and rapidly determine dipropylmalonic acid (A) and impurities (B, C, D, E, F and G) thereof, also can effectively separate and rapidly determine sodium valproate and a synthetic intermediate dipropylmalonic acid thereof, and can be widely applied to quality control of dipropylmalonic acid and quality evaluation of sodium valproate.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a method for detecting impurities related to dipropylmalonic acid. Background technique [0002] Dipropylmalonic acid is a pharmaceutical intermediate that often appears in the preparation process of sodium valproate raw material medicine. Sodium valproate (also known as sodium 2-propylvalerate, sodium dipropylacetate) is a sodium salt of saturated fatty acid. In 1963, the French Meurier first confirmed that this compound has antiepileptic effect. At present, sodium valproate is widely used in various types of epilepsy, absence seizures, tonic-clonic seizures, some refractory epilepsy, mania, depression and other clinical treatments. [0003] The synthetic route of sodium valproate reported in the prior art mainly uses dimethyl malonate (or diethyl malonate) and n-propane bromide as starting materials, and through alkylation and hydrolysis, the key intermediate dipropylene gly...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34
CPCG01N30/02G01N30/34
Inventor 刘泽荣徐金龙陈皓陈刚瞿春密董小峰
Owner SICHUAN CREDIT PHARMA