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Method for determining related impurities I of atorvastatin calcium

A technology of atorvastatin calcium and related impurities, which is applied in the detection field of pharmaceutical impurities to achieve the effect of improving the purity

Pending Publication Date: 2021-11-26
天津嘉林科医有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, atorvastatin calcium also contains other impurities, and the detection of other impurities is not mentioned in the relevant impurity detection standards of atorvastatin calcium. Therefore, it is necessary to continue research on other impurities to improve the quality of atorvastatin calcium. quality

Method used

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  • Method for determining related impurities I of atorvastatin calcium
  • Method for determining related impurities I of atorvastatin calcium
  • Method for determining related impurities I of atorvastatin calcium

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Experimental program
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Effect test

Embodiment 1

[0031] 1. HPLC chromatographic conditions Chromatographic column: Wondasil C18 (4.6mm×250mm, 5μm);

[0032] Mobile phase: mobile phase A is acetonitrile-tetrahydrofuran-acetate buffer, wherein the volume ratio of acetonitrile: tetrahydrofuran: acetate buffer is 35:3:62;

[0033] Mobile phase B is acetonitrile-tetrahydrofuran-acetate buffer, wherein the volume ratio of acetonitrile: tetrahydrofuran: acetate buffer is 82:3:15;

[0034] The preparation method of the acetic acid buffer solution is: take 1.50g of ammonium acetate, add 700mL of water to dissolve, after dissolving, adjust the pH to 4.0 with glacial acetic acid, then add water to 1000mL;

[0035] Flow rate: 1.0ml / min;

[0036] Detection wavelength: 244nm, column temperature 30°C;

[0037] Injection volume: 20μL;

[0038] The mobile phase gradient elution conditions are shown in Table 1.1.

[0039] Table 1.1 Mobile phase gradient elution conditions

[0040] time / min Mobile phase A / % Mobile phase B / % ...

Embodiment 2

[0052] 1. HPLC chromatographic conditions Chromatographic column: Wondasil C18 (4.6mm×250mm, 5μm);

[0053] Mobile phase: mobile phase A is acetonitrile-tetrahydrofuran-acetate buffer, wherein the volume ratio of acetonitrile: tetrahydrofuran: acetate buffer is 40:5:55;

[0054] Mobile phase B is acetonitrile-tetrahydrofuran-acetate buffer, wherein the volume ratio of acetonitrile: tetrahydrofuran: acetate buffer is 85:5:10;

[0055] The preparation method of the acetic acid buffer solution is: take 1.55g of ammonium acetate, add 800mL of water to dissolve, after dissolving, adjust the pH to 4.0 with glacial acetic acid, then add water to 1000mL;

[0056] Flow rate: 1.0ml / min;

[0057] Detection wavelength: 244nm, column temperature 30°C;

[0058] Injection volume: 20μL;

[0059] The mobile phase gradient elution conditions are shown in Table 2.1.

[0060] Table 2.1 Mobile phase gradient elution conditions

[0061] time / min Mobile phase A / % Mobile phase B / % ...

Embodiment 3

[0096] 1. HPLC chromatographic conditions Chromatographic column: Wondasil C18 (4.6mm×250mm, 5μm);

[0097] Mobile phase: mobile phase A is acetonitrile-tetrahydrofuran-acetate buffer, wherein the volume ratio of acetonitrile: tetrahydrofuran: acetate buffer is 45:7:48;

[0098] Mobile phase B is acetonitrile-tetrahydrofuran-acetate buffer solution, wherein the volume ratio of acetonitrile: tetrahydrofuran: acetate buffer solution is 87:7:6; the preparation method of acetate buffer solution is: take 1.58g ammonium acetate, add 900mL water for Dissolve, after dissolving, adjust the pH to 4.0 with glacial acetic acid, then add water to 1000mL;

[0099] Flow rate: 1.0ml / min;

[0100] Detection wavelength: 244nm, column temperature 30°C;

[0101] Injection volume: 20μL;

[0102] The mobile phase gradient elution conditions are shown in Table 3.1.

[0103] Table 3.1 Mobile phase gradient elution conditions

[0104] time / min Mobile phase A / % Mobile phase B / % 0...

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Abstract

The invention discloses a method for determining related impurities I of atorvastatin calcium, and belongs to the field of detection of drug impurities. The method comprises the following steps: (a) preparation of a test solution: weighing atorvastatin calcium, adding a solvent for dissolving, and quantitatively diluting to prepare a solution containing 0.8-1.2 mg of the atorvastatin calcium per 1mL as the test solution; (b) preparation of a mixed reference substance solution: weighing an impurity A reference substance, an impurity B reference substance, an impurity C reference substance, an impurity D reference substance, an impurity E reference substance, an impurity I reference substance and an atorvastatin calcium reference substance, adding the solvent for dissolving, and quantitatively diluting to prepare a solution containing 54-66 microgram of the impurity B, 5-15 microgram of the impurity A, 5-15 microgram of the impurity C, 5-15 microgram of the impurity D, 5-15 microgram of the impurity E, 5-15 microgram of the impurity I and 45-55 microgram of atorvastatin calcium in each 1mL; taking the solution as the mixed reference solution; and (C) analysis of the test solution and the mixed reference solution by adopting high performance liquid chromatography. The effect of detecting other impurities in atorvastatin calcium can be achieved.

Description

technical field [0001] The invention relates to the detection field of pharmaceutical impurities, in particular to a method for determining the impurity I related to atorvastatin calcium. Background technique [0002] Atorvastatin calcium usually exists in the form of trihydrate, its chemical name is: [R-(R*,R*,)]-2-(4-fluorophenyl)-β,δ-dihydroxy-5 Calcium -(1-methylethyl)-3-phenyl-4-[(aniline)carbonyl]-1-hydro-pyrrole-1-heptanoate trihydrate. [0003] There must be impurities in atorvastatin calcium during the synthesis process. The existence of impurities will affect the purity of the drug and also affect the drug properties of the drug. As the world's best-selling blood lipid-lowering drug, atorvastatin calcium must be strictly Control the content of impurities to ensure drug safety. The impurities and harmful substances produced in the preparation process can cause adverse reactions. Therefore, it is necessary to study the impurities in order to obtain higher quality at...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/74
CPCG01N30/02G01N30/06G01N30/74G01N2030/047
Inventor 陈海波赵凤新李欣怡耿宇瞳荣婉琪
Owner 天津嘉林科医有限公司
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