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Method for detecting pitavastatin calcium intermediate and impurities

A technology of pitavastatin calcium and detection method, which is applied in the field of drug detection and analysis, and can solve disadvantages and other problems

Pending Publication Date: 2022-04-08
苏州正济药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] In the prior art, there is no corresponding detection method for the above-mentioned intermediate and its five impurities, which is very unfavorable for (3R,5S,6E)-7-[2-cyclopropyl-4-(4-fluorophenyl) -3-quinolinyl]-3,5-dihydroxy-6-heptenoic acid methyl ester and pitavastatin calcium quality control, so an effective elution, separation and quantitative analysis and detection method for the pitavastatin calcium was established It is very necessary to detect and analyze the intermediates and impurities of Vastatin calcium

Method used

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  • Method for detecting pitavastatin calcium intermediate and impurities
  • Method for detecting pitavastatin calcium intermediate and impurities
  • Method for detecting pitavastatin calcium intermediate and impurities

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0040] Instrument: Agilent 1260

[0041] Chromatographic column: waters Symmetry C18 4.6×150mm, 3.5um

[0042] Mobile phase: Phase A: 10mmol / L potassium dihydrogen phosphate aqueous solution (phosphoric acid to adjust pH=3.2)

[0043] Phase B: Acetonitrile

[0044] Detection wavelength: 245nm

[0045] Flow rate: 1.0ml / min

[0046] Column temperature: 25°C

[0047] Injection volume: 10μl

[0048] Table 1. Gradient elution program of Example 1

[0049]

[0050]

[0051] Diluent (blank solution): acetonitrile.

[0052] Preparation of impurity localization solution: take appropriate amount of reference substances of impurity 1, impurity 2, impurity 3, impurity 4 and impurity 5, weigh them accurately, add acetonitrile to dissolve and dilute, and make the contents of impurity 1-5 in each 1ml are about Solutions of 0.9 μg, 0.45 μg, 0.3 μg, 0.1125 μg, and 0.3 μg were used as positioning solutions for impurities 1-5, respectively.

[0053] System suitability solution prep...

Embodiment 2

[0058] Instrument: Agilent 1260

[0059] Chromatographic column: SVEA phHex 4.6×250mm, 3.5um

[0060]Mobile phase: Phase A: 5mmol / L ammonium acetate buffer solution (adjust pH to 3.2 with phosphoric acid)

[0061] Phase B: Acetonitrile

[0062] Detection wavelength: 245nm

[0063] Flow rate: 0.8ml / min

[0064] Column temperature: 25°C

[0065] Injection volume: 10μl

[0066] Table 2. Gradient elution program of Example 2

[0067] Elution time (min) Phase A (%) Phase B (%) 0 55 45 5 55 45 30 45 55 45 10 90 60 10 90 60.1 55 45 75 55 45

[0068] Adopt the same method as Example 1 to prepare impurity positioning solution, system suitability solution, wherein the consumption of intermediates and impurities is shown in Table 3 below, adopt the same sample determination method as Example 1 to record the retention time of intermediates and impurities Also shown in Table 3 below.

[0069] Table 3. The positioning detect...

Embodiment 3

[0073] Instrument: Agilent 1260

[0074] Chromatographic column: Agilent ZORBAX SB-C8 4.6×150mm, 5μm;

[0075] Mobile phase: Phase A: 5mmol / L ammonium acetate buffer solution (adjust pH to 3.2 with phosphoric acid)

[0076] Phase B: Acetonitrile

[0077] Detection wavelength: 245nm

[0078] Flow rate: 1.0ml / min

[0079] Column temperature: 25°C

[0080] Injection volume: 10μl

[0081] Table 4. Gradient elution program of Example 3

[0082] Elution time (min) Phase A (%) Phase B (%) 0 55 45 5 55 45 20 50 50 30 10 90 37 10 90 37.1 55 45 45 55 45

[0083] Adopt the same method as Example 1 to prepare impurity localization solution, system suitability solution, wherein the consumption of intermediate and impurity is shown in Table 5 below, adopt the same sample determination method as Example 1 to record the retention time of intermediate and impurity Also shown in Table 5 below.

[0084] Table 5. The positioning d...

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Abstract

The invention provides a method for detecting pitavastatin calcium intermediates and impurities, which adopts high performance liquid chromatography to detect and analyze the pitavastatin calcium intermediates and impurities 1, 2, 3, 4 and 5, adopts octaalkylsilane bonded silica gel as a chromatographic column of a filling agent, adopts an ammonium acetate buffer solution as a mobile phase A, and adopts a mobile phase B to detect the pitavastatin calcium intermediates. Acetonitrile is used as a mobile phase B, and gradient elution is carried out. According to the method, known impurities can be accurately detected, the main peak of the intermediate and the peak of the known impurities can be effectively separated, and the method is a brand-new detection and analysis method beneficial to quality control of the pitavastatin calcium intermediate.

Description

technical field [0001] The invention relates to the technical field of drug detection and analysis, in particular to a method for detecting pitavastatin calcium intermediates and impurities. Background technique [0002] Pitavastatin calcium, the chemical name is (+)-bis{(3R,5S,6E)-7-[2-cyclopropyl-4-(fluorophenyl)quinoline-3-phenyl]-3, 5-Dihydroxy-6-heptenoic acid} calcium salt (2:1), is the third-generation statin drug jointly developed by Nippon Chemical Industry Co., Ltd. and Kowa Co., Ltd., which was launched in Japan in September 2003. In 2009 On March 27, 2010, the generic drug Pitavastatin Calcium Tablets (trade name: Guanshuang) launched by Beijing Shuanghe Pharmaceutical Co., Ltd. was launched in my country. Pitavastatin calcium, as a hydroxymethylglutaryl coenzyme A (HMG-CoA) reductase inhibitor, has the effect of significantly reducing low-density lipoprotein cholesterol (LDL-C). Currently one of the statin drugs with better blood lipid-lowering effect in interna...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34
CPCY02P20/55
Inventor 梁燕娜邓瑜
Owner 苏州正济药业有限公司
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