Method for separating and measuring content of optical isomers in tartaric acid

A technology for optical isomers and tartaric acid, applied in the field of chemical analysis, can solve problems such as high cost and complicated detection process

Pending Publication Date: 2022-02-18
WUHAN WUYAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Method for separating and measuring content of optical isomers in tartaric acid
  • Method for separating and measuring content of optical isomers in tartaric acid
  • Method for separating and measuring content of optical isomers in tartaric acid

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Embodiment 1

[0053] 1. Chromatographic conditions:

[0054] Chromatographic column: CHIRALPAK AD-H 4.6×250mm, 5μm

[0055] Stationary phase: Amylose-tris[3,5-dimethylcarbamate] derivative

[0056] Mobile phase: Measure 850ml of n-hexane, 150ml of isopropanol, 10ml of tert-butanol, 2ml of trifluoroacetic acid, mix well, and elute isocratic

[0057] Column temperature: 25°C

[0058] Mobile phase flow rate: 0.8ml / min

[0059] Detection wavelength: 223nm

[0060] Injection volume: 20μL

[0061] 2. Experimental steps

[0062]1) Take an appropriate amount of tartaric acid sample, dissolve it with ethanol, and prepare a solution containing 10 mg of tartaric acid sample per 1 ml, then dilute with mobile phase to a solution of 5 mg per 1 ml of tartaric acid sample;

[0063] 2) Take 20 μl of the sample solution obtained in step 1) and inject it into a high-performance liquid chromatograph, and record the chromatogram. attached figure 1 The experimental results show that peak No. 1 is D-tarta...

Embodiment 2

[0065] 1. Chromatographic conditions:

[0066] Chromatographic column: CHIRALPAK AD-H 4.6×250mm, 5μm

[0067] Stationary phase: Amylose-tris[3,5-dimethylcarbamate] derivative

[0068] Mobile phase: Measure 830ml of n-hexane, 170ml of isopropanol, 10ml of tert-butanol, 2ml of trifluoroacetic acid, mix well, and elute isocratic

[0069] Column temperature: 25°C

[0070] Mobile phase flow rate: 0.8ml / min

[0071] Detection wavelength: 223nm

[0072] Injection volume: 20μL

[0073] 2. Experimental steps

[0074] 1) Take an appropriate amount of tartaric acid sample, dissolve it with ethanol, and prepare a solution containing 10 mg of tartaric acid sample per 1 ml, then dilute with mobile phase to a solution of 5 mg per 1 ml of tartaric acid sample;

[0075] 2) Take 20 μl of the sample solution obtained in step 1) and inject it into a high-performance liquid chromatograph, and record the chromatogram. attached figure 2 The experimental results show that peak No. 1 is D-tar...

Embodiment 3

[0077] 1. Chromatographic conditions:

[0078] Chromatographic column: CHIRALPAK AD-H 4.6×250mm, 5μm

[0079] Stationary phase: Amylose-tris[3,5-dimethylcarbamate] derivative

[0080] Mobile phase: Measure 880ml of n-hexane, 120ml of isopropanol, 10ml of tert-butanol, 2ml of trifluoroacetic acid, mix well, and elute isocratic

[0081] Column temperature: 25°C

[0082] Mobile phase flow rate: 0.8ml / min

[0083] Detection wavelength: 223nm

[0084] Injection volume: 20μL

[0085] 2. Experimental steps

[0086] 1) Take an appropriate amount of tartaric acid sample, dissolve it with ethanol, and prepare a solution containing 10 mg of tartaric acid sample per 1 ml, then dilute with mobile phase to a solution of 5 mg per 1 ml of tartaric acid sample;

[0087] 2) Take 20 μl of the sample solution obtained in step 1) and inject it into a high-performance liquid chromatograph, and record the chromatogram. attached image 3 The experimental results show that peak No. 1 is D-tart...

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Abstract

The invention relates to the technical field of chemical analysis, in particular to a method for separating and determining the content of optical isomers in tartaric acid. The invention provides a method for separating and determining the content of optical isomers in tartaric acid, which is carried out by using high performance liquid chromatography, and the analysis conditions are as follows: an amylose-tri [3, 5-dimethyl carbamate] derivative is used as a stationary phase; and L-tartaric acid and D-tartaric acid can be simply and quickly separated very well by taking n-hexane, isopropanol, tert-butyl alcohol and trifluoroacetic acid as mobile phases and performing isocratic elution, and the contents of the L-tartaric acid and the D-tartaric acid are measured.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for separating and measuring the content of tartaric acid optical isomers. Background technique [0002] Tartaric acid exists in three optical isomers: levo-tartaric acid (D-tartaric acid), dextro-tartaric acid (L-tartaric acid) and meso-tartaric acid (meso-tartaric acid). Equal moles of L-tartaric acid and D-tartaric acid are mixed to form racemic tartaric acid. In the field of medicine, the control of the impurity content of raw materials is also one of the key steps in the quality control of medicines. In order to improve the production quality of medicines, it is necessary to analyze and detect the relative content of L-tartaric acid and D-tartaric acid in tartaric acid samples, but at present, there is no relatively simple and mature method for the separation and detection of tartaric acid optical isomers. [0003] Patent CN109738560A in the prior art di...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34
CPCG01N30/02G01N30/06G01N30/34
Inventor 赵涛涛万文标王成洪健王浩张召忠张琦
Owner WUHAN WUYAO PHARMA
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