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High performance liquid chromatography (HPLC) purity detection method for completely separating 2-cyano-4-pyridine carboxylic acid methyl ester from major impurities of 2-cyano-4-pyridine carboxylic acid methyl ester

A technology of methyl pyridinecarboxylate and high performance liquid chromatography, applied in the field of high performance liquid chromatography detection, can solve problems such as being difficult to inquire

Inactive Publication Date: 2016-11-16
江苏悦兴医药技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to completely separate methyl 2-cyano-4-pyridinecarboxylate from its main impurity peak, improve the peak shape, and accurately control the content of methyl 2-cyano-4-pyridinecarboxylate, it is currently difficult to find 2 - Correlative HPLC method for complete separation of methyl cyano-4-pyridinecarboxylate and its major impurity peaks

Method used

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  • High performance liquid chromatography (HPLC) purity detection method for completely separating 2-cyano-4-pyridine carboxylic acid methyl ester from major impurities of 2-cyano-4-pyridine carboxylic acid methyl ester
  • High performance liquid chromatography (HPLC) purity detection method for completely separating 2-cyano-4-pyridine carboxylic acid methyl ester from major impurities of 2-cyano-4-pyridine carboxylic acid methyl ester
  • High performance liquid chromatography (HPLC) purity detection method for completely separating 2-cyano-4-pyridine carboxylic acid methyl ester from major impurities of 2-cyano-4-pyridine carboxylic acid methyl ester

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Experimental program
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Effect test

Embodiment 1

[0049] The high-performance liquid chromatography detection method of 2-cyano-4-pyridinecarboxylate methyl ester:

[0050] (1) Preparation of the test solution: Accurately weigh 10 mg of methyl 2-cyano-4-pyridinecarboxylate, place it in a 10 ml volumetric flask, add mobile phase to dissolve and dilute to the mark, shake well, and make a concentration of 1 mg / ml solution, as the test solution;

[0051] Preparation of impurity reference substance solution A: Accurately weigh 10 mg of isonicotinic acid methyl ester, put it in a 10ml volumetric flask, add mobile phase to dissolve and dilute to the mark, shake well, and make a solution with a concentration of 1 mg / ml to obtain an impurity reference substance solution A: Take another 10 mg of methylisonicotinic acid N-oxide, put it in a 10 ml volumetric flask, add mobile phase to dissolve and dilute to the mark, shake well, and make a solution with a concentration of 1 mg / ml to obtain impurity reference substance solution B;

[00...

Embodiment 2

[0073] Except that the mobile phase was changed to methanol-5mmol sodium hexanesulfonate (28:72, volume ratio) in the detection conditions, other conditions were the same as in Example 1.

[0074] According to the above conditions, take 20ul of the system suitability solution and inject it into the liquid chromatograph, record the chromatogram, see the attached figure 2 and Table 2.

[0075] Accurately measure 20 ul of the test solution, inject it into the liquid chromatograph, record the chromatogram, and calculate the content of methyl isonicotinate in the test product by the peak area normalization method to be 0.01%, methyl isonicotinic acid N-oxide The content is 0.01%.

[0076] Table 2, separation effect of methyl isonicotinate, methyl isonicotinic acid N-oxide and methyl 2-cyano-4-pyridinecarboxylate under the conditions of Example 2.

[0077] Chromatographic peak

[0078] The results show that the separation degree of methyl isonicotinate and 2-cyano-4-pyr...

Embodiment 3

[0080] Except that the mobile phase was changed to methanol-5mmol sodium hexanesulfonate (32:68, volume ratio) in the detection conditions, other conditions were the same as in Example 1.

[0081] According to the above conditions, take 20ul of the system suitability solution and inject it into the liquid chromatograph, record the chromatogram, see the attached image 3 and Table 3.

[0082] Accurately measure 20 ul of the test solution, inject it into the liquid chromatograph, record the chromatogram, and calculate the content of methyl isonicotinate in the test product by the peak area normalization method to be 0.01%, methyl isonicotinic acid N-oxide Content is 0.01%

[0083] Table 3, separation effect of methyl isonicotinate, methyl isonicotinic acid N-oxide and methyl 2-cyano-4-pyridinecarboxylate under the conditions of Example 3.

[0084] Chromatographic peak

[0085] The results show that the separation degree of methyl isonicotinate and 2-cyano-4-pyridinec...

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Abstract

The invention discloses a high performance liquid chromatography (HPLC) purity detection method for completely separating 2-cyano-4-pyridine carboxylic acid methyl ester from major impurities. The method comprises the following steps: a. preparing a test solution; b. preparing a reference solution; c. detecting the test solution and the reference solution respectively by adopting HPLC, wherein the detection conditions are as follows: the chromatographic column is an ODS-C18 column; the mobile phases are buffer salt and methanol; the injection volume is 20mu l; the flow rate is 0.5-1.5ml / min; the column temperature is 10-40 DEG C; the detection wavelength is 200-300nm. The method achieves complete separation of 2-cyano-4-pyridine carboxylic acid methyl ester and the major impurities under the normal temperature condition by way of isocratic elution and achieves accurate control of the content of 2-cyano-4-pyridine carboxylic acid methyl ester.

Description

technical field [0001] The invention relates to a high performance liquid chromatography detection method, in particular to a high performance liquid chromatography analysis method for separating methyl 2-cyano-4-pyridinecarboxylate and its main impurities by means of isocratic elution. Background technique [0002] Tobicistat is used to treat chronic hyperuricemia of gout. Compared with the traditional drug allopurinol (purine analogue), tobicistat will not affect the metabolism of purine and pyridine and the activity of its enzymes, and its effect on reducing uric acid is stronger. Do not need large doses of repeated administration, better security, and methyl 2-cyano-4-pyridinecarboxylate is an important raw material for the synthesis of tobicistat, the molecular formula of methyl 2-cyano-4-pyridinecarboxylate :C 8 h 6 N 2 o 2 , its structural formula is as follows: [0003] [0004] The impurities produced during the synthesis of methyl 2-cyano-4-pyridinecarboxyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 陈润翟富民陆学山徐小丹包华兰陈建丽
Owner 江苏悦兴医药技术有限公司
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