Separation and/or detection method of impurities in atorvastatin calcium

A technology of atorvastatin calcium and atorvastatin is applied in the field of separation or detection of atorvastatin calcium enantiomer and atorvastatin calcium lactone, which can solve the problem that the accuracy of detection results cannot be guaranteed , can not be effectively separated and other problems, to improve the quality and safety of drugs, the effect of good separation effect

Inactive Publication Date: 2020-01-03
北京伟林恒昌医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

All do not relate to the separation and detection method of atorvastatin calcium enantiomer and impurity H in atorvastatin calcium in the prior art, in reference quality standard: USP40Atorvastatin Calcium (P2898) and atorvastatin import In the registration standard (JX20120157), high-performance liquid chromatography is used for separation, and the mobile phase is n-hexane-absolute ethanol-acidic compound, mixed according to a certain ratio, and prepared. According to the method in the above-mentioned standard, atorvastatin calcium Impurity H and enantiomers cannot be effectively separated, and the accuracy of the test results cannot be guaranteed

Method used

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  • Separation and/or detection method of impurities in atorvastatin calcium
  • Separation and/or detection method of impurities in atorvastatin calcium
  • Separation and/or detection method of impurities in atorvastatin calcium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Testing instruments and chromatographic conditions

[0068] Detection instrument: high performance liquid chromatography

[0069] Chromatographic conditions: the chromatographic column is a chiral chromatographic column of polysaccharide derivatives, the column temperature is 35°C, an ultraviolet detector is used, and the detection wavelength is set to 244nm; the flow rate of the mobile phase is 1ml / min; the volume ratio is 850:150: 1 of n-hexane-absolute ethanol-trifluoroacetic acid is the mobile equal degree elution.

[0070] Preparation of atorvastatin calcium impurity H positioning solution: Weigh an appropriate amount of atorvastatin calcium impurity H, add solvent to dissolve and dilute to the scale, so that the concentration of atorvastatin calcium impurity H is 0.002mg / mL, filter, and the solvent Methanol-absolute ethanol-n-hexane with a volume ratio of 1:1:3;

[0071] Preparation of atorvastatin calcium enantiomer localization solution: Weigh an appropriate a...

Embodiment 2

[0078] Testing instruments and chromatographic conditions

[0079] Detection instrument: high performance liquid chromatography

[0080] Chromatographic conditions: the chromatographic column is a chiral chromatographic column of polysaccharide derivatives, the column temperature is 35°C, an ultraviolet detector is used, and the detection wavelength is set to 244nm; the flow rate of the mobile phase is 1ml / min; the volume ratio is 95:2: 3: 0.2: 0.2 n-hexane-methanol-absolute ethanol-formic acid-diethylamine is the mobile equal degree elution.

[0081] Blank excipient solution: add atorvastatin calcium blank excipient to the solvent accounting for 50% of the total volume of the test sample solution, shake fully to dissolve atorvastatin, add solvent to constant volume, so that the concentration of blank excipient is equivalent to that of atorvastatin Statin calcium 1 mg / mL, filtered, wherein the solvent is methanol-absolute ethanol-n-hexane with a volume ratio of 1:1:3.

[008...

Embodiment 3

[0087] Testing instruments and chromatographic conditions

[0088] Detection instrument: high performance liquid chromatography

[0089] Chromatographic conditions: the chromatographic column is a chiral chromatographic column of polysaccharide derivatives, the column temperature is 35°C, an ultraviolet detector is used, and the detection wavelength is set to 244nm; the flow rate of the mobile phase is 1ml / min; the volume ratio is 95:2: 3: 0.1:0.1 n-hexane-methanol-absolute ethanol: trifluoroacetic acid: triethylamine for mobile equipotential elution.

[0090] The preparation of the system suitability solution in this example is the same as in Example 1.

[0091] Take 20 μl of the system suitability solution, inject it into the liquid chromatograph, measure it according to the chromatographic conditions, record the chromatogram, and complete the determination; the obtained chromatogram is as follows: Figure 7 shown.

[0092]The results showed that: atorvastatin calcium ena...

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Abstract

The invention relates to a separation and/or detection method of impurities in atorvastatin calcium. The impurities are atorvastatin calcium enantiomers and/or atorvastatin calcium lactone (impurity H). The method uses high-performance liquid chromatography for separation or detection. A mobile phase of the high-performance liquid chromatography is monohydric alcohol-organic acid-organic base of n-hexane-C1-C6. A volume ratio of the monohydric alcohol-organic acid-organic base of the n-hexane-C1-C6 is 85-98:2-15:0.05-0.5:0.05-0.5. The method can realize effective separation on the three partsof the atorvastatin calcium, the atorvastatin calcium enantiomers and the atorvastatin calcium lactone; and at the same time, the method of the invention can be used for detection of the atorvastatincalcium enantiomers and the atorvastatin calcium lactone, and can effectively improve medicine quality and safety of the atorvastatin calcium.

Description

technical field [0001] The invention belongs to the technical field of biomedicine, and in particular relates to a method for separating or detecting atorvastatin calcium enantiomers and atorvastatin calcium lactone (impurity H). Background technique [0002] Atorvastatin calcium is the third-generation statin blood lipid-regulating drug. It is a selective and competitive inhibitor of HMG-CoA reductase. Acid monoacyl-CoA reductase) and cholesterol synthesis, thereby reducing plasma cholesterol and lipoprotein levels, and by increasing the liver LDL receptors on the cell surface to enhance the uptake and metabolism of LDL. [0003] Atorvastatin calcium is a blood lipid-lowering drug widely used in clinical practice. It can inhibit the synthesis of low-density lipoprotein and cholesterol in the body by inhibiting HMG-CoA reductase, so as to achieve the purpose of lowering blood lipids. There are two chiral centers in the molecular structure of atorvastatin calcium, so there a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14
CPCG01N30/02G01N30/14
Inventor 曹相林李萍张国芳胡兰萍商丹丹吴绪丽
Owner 北京伟林恒昌医药科技有限公司
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