Determination method of related substances in atorvastatin calcium capsules

A technology for the detection of atorvastatin calcium, which is applied in the field of separation of drugs into components for testing or analysis by column chromatography, which can solve problems such as threats to clinical drug safety and achieve the effect of improving quality standards

Active Publication Date: 2011-12-14
北京汉典中西药研究开发中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the quality standards of atorvastatin calcium capsules that have been on the market only stipulate the detection method of the total amount of relat...

Method used

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  • Determination method of related substances in atorvastatin calcium capsules
  • Determination method of related substances in atorvastatin calcium capsules
  • Determination method of related substances in atorvastatin calcium capsules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Embodiment 1 The establishment of detection method

[0074] 1 Chromatographic conditions

[0075] A Kromasil C-18 chromatographic column was selected, with a particle size of 5 μm, a column length of 250 mm, and a column diameter of 4.6 mm, using an Agilent 1200 chromatographic workstation.

[0076] With acetonitrile-tetrahydrofuran (92.5:7.5, v / v) as mobile phase A, 0.56% ammonium dihydrogen phosphate solution-mobile phase A (58:42, v / v) as mobile phase B, 0.56% ammonium dihydrogen phosphate solution -Mobile phase A-methanol (100:100:300, v / v) is used as mobile phase C, the detection wavelength is 246nm, the column temperature is 25°C, and the elution conditions are:

[0077] From 0 min to 20 min, the mobile phase is B, and the flow rate is 1.8ml / min; from the 20 min to the 35 min, the mobile phase gradient changes to B and C with a volume ratio of 25%:75%, B+C=100%, and the flow rate 1.5ml / min; from the 35th minute to the 40th minute, keep the proportion of the mobi...

Embodiment 2

[0105]Adopt Kromasil C-18 chromatographic column, particle diameter 5 μm, column length 250mm, column diameter 4.6mm; Adopt Agilent 1100 chromatographic workstation; With acetonitrile-tetrahydrofuran (92:8, v / v) as mobile phase A, 0.56% dihydrogen phosphate Ammonium solution-mobile phase A (56:44, v / v) was used as mobile phase B, 0.56% ammonium dihydrogen phosphate solution-mobile phase A-methanol (100:100:300, v / v) was used as mobile phase C, according to The following table carries out gradient elution, the detection wavelength is 240nm, and the column temperature is 20°C, wherein 0.56% in 0.56% ammonium dihydrogen phosphate solution refers to the mass volume ratio, and the elution conditions are as follows:

[0106] From 0 min to 17 min, the mobile phase is B, and the flow rate is 1.8ml / min; from 17 min to 32 min, the mobile phase gradient changes to B and C with a volume ratio of 25%:75%, B+C=100%, and the flow rate 1.5ml / min; from the 32nd to the 40th minute, keep the rat...

Embodiment 3

[0112] Adopt Discovery C-18 chromatographic column, particle diameter 5 μm, column length 250mm, column diameter 4.6mm; Adopt Shimadzu LC-2010AHT chromatographic workstation; With acetonitrile-tetrahydrofuran (95:5, v / v) as mobile phase A, 0.56% Ammonium dihydrogen phosphate solution-mobile phase A (60:40, v / v) as mobile phase B, 0.56% ammonium dihydrogen phosphate solution-mobile phase A-methanol (100:100:300, v / v) as mobile phase C, carry out gradient elution, detection wavelength is 250nm, column temperature is 30 ℃, wherein 0.56% in 0.56% ammonium dihydrogen phosphate solution refers to mass volume ratio, and elution condition is as follows:

[0113] From 0 min to 20 min, the mobile phase is B, and the flow rate is 1.8ml / min; from the 20 min to the 35 min, the mobile phase gradient changes to B and C with a volume ratio of 22%:78%, B+C=100%, and the flow rate From the 35th minute to the 41st minute, keep the ratio of the mobile phase unchanged, and the flow rate is 1.5ml / m...

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Abstract

A detection method of atorvastatin calcium capsule related substances of the invention relates to a method which tests or analyzes a drug by separating the drug into various components by adsorption, and the method can detect a single component of related substances in an atorvastatin calcium capsule, and facilitates the improvement of quality standard of atorvastatin calcium capsules. According to the invention, a sample solution to be tested, a self-control solution, and a blank solution are weighed; the solutions are injected into a liquid chromatography, wherein the chromatographic conditions are as follows: a chromatographic column with octadecyl silane bonded silica as a filler is selected; acetonitrile-tetrahydrofuran is used as a mobile phase A; 0.56% ammonium biphosphate solution-mobile phase A is used as a mobile phase B; 0.56% ammonium biphosphate solution- mobile phase A-methanol is used as a mobile phase C; gradient elution is performed; the detection wavelength is 240-250 nm, and the column temperature is 20 DEG C-30 DEG C, wherein in the 0.56% ammonium biphosphate solution, 0.56% is a mass-volume ratio; and a chromatogram is recorded.

Description

technical field [0001] The invention relates to a method for testing or analyzing drugs by separating them into components by adsorption, in particular to a method for testing or analyzing drugs by separating them into components by using column chromatography. Background technique [0002] Atorvastatin Calcium is a lipid-regulating drug suitable for patients with primary hypercholesterolemia. At present, the quality standards of atorvastatin calcium capsules that have been on the market only stipulate the detection method of the total amount of related substances, and do not specify the detection method of a single component of related substances, which poses a potential threat to the safety of clinical medication. Contents of the invention [0003] The invention provides a method for detecting the single component and the total amount of related substances in atorvastatin calcium capsules. [0004] The detection method of atorvastatin calcium capsule related substance o...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 林德良
Owner 北京汉典中西药研究开发中心
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