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High performance liquid chromatography of 3-tert-butyl dimethyl silica glutaric anhydride

A technology of tert-butyldimethylsiloxyglutaric anhydride and high performance liquid chromatography, which is applied in the field of high performance liquid chromatography, can solve the problems of lack of control of degradation products, inability to detect interference, etc. Simple to use effects

Active Publication Date: 2013-06-05
EMEISHAN HONGSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The invention relates to a high-performance liquid chromatography analysis method for 3-tert-butyldimethylsiloxyglutaric anhydride, which solves the shortcomings of the lack of control of the degradation products of 3-tert-butyldimethylsiloxyglutaric anhydride in the prior art , and the problem of being unable to detect the interference of unknown impurities on 3-tert-butyldimethylsiloxyglutaric anhydride

Method used

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  • High performance liquid chromatography of 3-tert-butyl dimethyl silica glutaric anhydride
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  • High performance liquid chromatography of 3-tert-butyl dimethyl silica glutaric anhydride

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Embodiment 1

[0031] The required instruments and conditions of this embodiment are as follows:

[0032] High performance liquid chromatography: Dalian Elite P1201, UV detector;

[0033] Chromatographic column: C18, 4.6×250mm, 3.5μm;

[0034] Buffer solution: Weigh 1.4g of potassium dihydrogen phosphate and dissolve it in 1L of water, adjust the pH to 2.2 with phosphoric acid, and filter;

[0035] Mobile phase: methanol-phosphate buffer; flow rate: 1.2mL / min; detection wavelength: 205nm; column temperature: 40°C; injection volume: 20μL.

[0036] Specific steps are as follows:

[0037] (1) Take an appropriate amount of 3-tert-butyldimethylsiloxyglutaric anhydride sample, dissolve it with methanol for 15 minutes sonication, and prepare a 3-tert-butyldimethylsiloxyglutaric anhydride sample with a concentration of 0.5mg / mL The solution was then centrifuged, and the supernatant was taken as the sample solution.

[0038] (2) Take 20 μL of the above sample solution and inject it into a liquid ...

Embodiment 2

[0041] The required instruments and conditions of this embodiment are as follows:

[0042] High performance liquid chromatography: Dalian Elite P1201, UV detector;

[0043] Chromatographic column: C18, 4.6×250mm, 3.5μm;

[0044] Buffer solution: Weigh 1.4g of ammonium dihydrogen phosphate and dissolve it in 1L of water, adjust the pH to 2.4 with phosphoric acid, and filter;

[0045] Mobile phase: methanol-phosphate buffer; flow rate: 1.0 mL / min; detection wavelength: 205 nm; column temperature: 30°C; injection volume: 20 μL.

[0046] Specific steps are as follows:

[0047] (1) Take an appropriate amount of 3-tert-butyldimethylsiloxyglutaric anhydride, dissolve it with home-made ultrasound, and make a 3-tert-butyldimethylsiloxyglutaric anhydride sample solution with a concentration of 0.5mg / mL , and then centrifuged, and the supernatant was taken as the sample solution.

[0048] (2) Take 20 μL of the above sample solution and inject it into a liquid chromatograph, use metha...

Embodiment 3

[0051] The required instruments and conditions of this embodiment are as follows:

[0052] High performance liquid chromatography: Dalian Elite P1201, UA detector;

[0053] Chromatographic column: C18, 4.6×250mm, 3.5μm;

[0054] Buffer solution: Weigh 1.4g of ammonium dihydrogen phosphate and dissolve it in 1L of water, adjust the pH to 2.4 with phosphoric acid, and filter;

[0055] Mobile phase: methanol-phosphate buffer; flow rate: 1.0 mL / min; detection wavelength: 205 nm; column temperature: 30°C; injection volume: 20 μL.

[0056] Specific steps are as follows:

[0057] (1) Prepare samples for alkali damage, acid damage, and oxidation damage:

[0058] Alkali destruction: Take an appropriate amount of 3-tert-butyldimethylsiloxyglutaric anhydride sample into a 10mL volumetric flask, add 2mL of 1N sodium hydroxide solution, leave it at room temperature for half an hour, add 1N hydrochloric acid to neutralize it, and prepare it with methanol 3-tert-butyldimethylsiloxyglutar...

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Abstract

The invention discloses a high performance liquid chromatography of 3-tert-butyl dimethyl silica glutaric anhydride and aims to solve the problems that degradation products of the 3-tert-butyl dimethyl silica glutaric anhydride are lack of control and interference of unknown impurities on the 3-tert-butyl dimethyl silica glutaric anhydride can not be detected in the prior art. The high performance liquid chromatography includes the following steps: 1, raw material 3-tert-butyl dimethyl silica glutaric anhydride is prepared into a sample solution with concentration of 0.1-1mg / ml; 2, 2 nm L-50 nm L of the sample solution is added in a liquid chromatograph; 3, a reversed phase column is used for isocratic elution with methyl alcohol and buffer salt with the pH 2-7 as mobile phase, the flow velocity is 0.5ml / min-1.5ml / min, and the detection wavelength is 210nm-260nm. The high performance liquid chromatography is simple and repeatable in operation, has the advantages of separating different chaff interferents, and is suitable for popularization.

Description

technical field [0001] The invention relates to a high performance liquid chromatography analysis method, in particular to a high performance liquid chromatography analysis method of 3-tert-butyldimethylsiloxy glutaric anhydride. Background technique [0002] 3-tert-butyldimethylsiloxy glutaric anhydride is the key starting material for the synthesis of rosuvastatin calcium, and its structural formula is: [0003] ; [0004] Yet the quality of 3-tert-butyldimethylsiloxy glutaric anhydride directly affects the quality of its synthesized rosuvastatin calcium, which in turn has a greater impact on the curative effect of the medicine. In order to ensure the quality of the synthesized rosuvastatin calcium, it is necessary to establish a relatively complete method for detecting the content of 3-tert-butyldimethylsiloxyglutaric anhydride. At present, there is no published detection method for the content of (3R)-tert-butyldimethylsilyloxy-5-oxo-6-triphenylphosphine hexanoic aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
Inventor 何海兵葛邵勇景红梅吴绪娇涂亮余泽民高斌
Owner EMEISHAN HONGSHENG PHARMA
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