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Preparation detection method for substances related to rosuvastatin calcium preparation

A technology of rosuvastatin calcium and rosuvastatin, applied in the field of medicine

Inactive Publication Date: 2014-05-07
RUNZE PHARMACEUTICAL (SUZHOU) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the pharmacopoeias of various countries consulted, there is no pharmacopoeia to control the quality of the above 8 impurities in rosuvastatin calcium preparations

Method used

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  • Preparation detection method for substances related to rosuvastatin calcium preparation
  • Preparation detection method for substances related to rosuvastatin calcium preparation
  • Preparation detection method for substances related to rosuvastatin calcium preparation

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0061] Preparation of Impurity 1, Impurity 3, and Impurity 4:

[0062] Take 0.5g of rosuvastatin calcium raw material, put it in a 50ml measuring bottle, add 2ml of 7mol / L hydrochloric acid solution, dissolve it with 50% acetonitrile solution and set the volume to the mark, shake well, place it in a water bath at 60°C for 0.5h, take it out, Let cool and use as stock solution 1.

[0063] Preparation of Impurity 2:

[0064] Take 0.5g of rosuvastatin calcium raw material, put it in a weighing bottle, heat it at 105°C for 7 days, let it cool, and use 50% acetonitrile solution to prepare rosuvastatin calcium raw material containing about 0.01g / ml per 1ml solution, as stock solution 2.

[0065] Preparation of impurity 5 and impurity 6:

[0066] Take 0.5g of rosuvastatin calcium raw material, put it in a 50ml measuring bottle, add 50% acetonitrile solution to dissolve and adjust the volume to the mark, shake well, put it under natural light for 4h, and use it as stock solution 3. ...

Embodiment 1

[0090] Instruments and reagents

[0091] Agilent1260 series high performance liquid chromatography; Sartorius CP225D analytical balance (1 / 100,000 grade); impurity reference substances: ①(3S,5S)-Rosuvastatin calcium diastereoisomers, ②Rosuvastatin- 5S-lactone, ③ rosuvastatin-5R-lactone, ④ rosuvastatin-5-oxidation, ⑤ rosuvastatin photodegradation product 1, ⑥ rosuvastatin photodegradation product 2, ⑦ rosuvastatin Statin photodegradation product 1-lactone, ⑧ rosuvastatin photodegradation product 2-lactone, self-made, purity ≥ 95%; rosuvastatin calcium tablets (self-made): batch number: 20130826 / 10mg.

[0092] Chromatographic conditions:

[0093] Agilent Zorbax extend-C18 (4.6*250mm, 5μm); with 0.05M sodium dihydrogen phosphate buffer (adjust pH to 2.0 with phosphoric acid): acetonitrile:methanol=46:20:34; detection wavelength: 242nm; column temperature: 40 °C; flow rate: 0.7ml / min; injection volume: 10μl.

[0094] Sample Preparation:

[0095] Preparation of reference substa...

Embodiment 2

[0102] Instruments and reagents

[0103] Agilent1260 series high performance liquid chromatography; Sartorius CP225D analytical balance (1 / 100,000 grade); impurity reference substances: ①(3S,5S)-Rosuvastatin calcium diastereoisomers, ②Rosuvastatin- 5S-lactone, ③ rosuvastatin-5R-lactone, ④ rosuvastatin-5-oxidation, ⑤ rosuvastatin photodegradation product 1, ⑥ rosuvastatin photodegradation product 2, ⑦ rosuvastatin Statin photodegradation product 1-lactone, ⑧ rosuvastatin photodegradation product 2-lactone, self-made, purity ≥ 95%; rosuvastatin calcium capsule (self-made): batch number: F6-144015 / 10mg.

[0104] Chromatographic conditions:

[0105] Agilent Zorbax extend-C18 (4.6*250mm, 5μm); with 0.05M sodium dihydrogen phosphate buffer (adjust pH to 2.0 with phosphoric acid): acetonitrile:methanol=46:20:34; detection wavelength: 242nm; column temperature: 40 °C; flow rate: 0.7ml / min; injection volume: 10μl.

[0106] Sample Preparation:

[0107] Preparation of reference subst...

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Abstract

The invention relates to a preparation detection method for substances related to rosuvastatin calcium preparation. The preparation detection method comprises the following steps: preparing (3S,5S)-rosuvastatin calcium diastereoisomer, rosuvastatin-5S-lactone, rosuvastatin-5R-lactone, rosuvastatin-5-oxide, a rosuvastatin photodegradation product 1, a rosuvastatin photodegradation product 2, rosuvastatin photodegradation product 1-lactone and rosuvastatin photodegradation product 2-lactone, which are used as comparison products of the substances related the rosuvastatin calcium preparation; metering a test sample solution, a comparison product solution and a blank solution; and injecting the solutions into a liquid chromatograph respectively. The chromatographic conditions are as follows: a chromatographic column is a C18 chromatographic column; the column temperature is 30-40 DEG C, the flow speed is 0.6-1.0ml / min and the detection wavelength is 210-260nm. The content of the substances related to the rosuvastatin calcium preparation can be detected so as to be good for improving the quality standard of the rosuvastatin calcium preparation.

Description

technical field [0001] The invention relates to a rosuvastatin calcium preparation used for treating hyperlipidemia, in particular to a preparation and detection method for related substances of the rosuvastatin calcium preparation, and belongs to the technical field of medicine. Background technique [0002] Rosuvastatin calcium (rosuvastatin calcium) is a selective HMG-CoA reductase inhibitor, suitable for primary hypercholesterolemia (type Ⅱa, including heterozygous familial hypercholesterolemia) or mixed lipemia Adjunctive therapy in patients with disorder (Type IIb) when diet or exercise regimens are suboptimal. Its chemical name is bis-[E-7-[4-(4-fluorophenyl)-6-isopropyl-2-[methyl(methylsulfonyl)amino]-pyrimidin-5-yl](3R ,5S)-3,5-dihydroxyhept-6-enoic acid] calcium salt (2:1), molecular formula C 44 h 54 CaF 2 N 6 o 12 S 2 , the chemical structure is as follows: [0003] [0004] During the preparation process of rosuvastatin calcium, due to the influence o...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/74
Inventor 蔡垠武利苗艳周志亮朱金莲夏晓琴
Owner RUNZE PHARMACEUTICAL (SUZHOU) CO LTD
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