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Analysis detection method of 2-(tert-butyldimethylsilyl oxyl)ethanol

A technology of tert-butyldimethylsilyloxy and detection method, which is applied in the field of high performance liquid chromatography analysis, and can solve the problems of inapplicability to the analysis and detection of 2-(tert-butyldimethylsilyloxy)ethanol and the like , to achieve stable and reliable results, simple operation and high sensitivity

Active Publication Date: 2016-11-23
SHANDONG NEWTIME PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although patents WO2012103959A1 and CN101175760A describe the analytical methods of everolimus and rapamycin-related derivatives, these methods are not suitable for the analysis and detection of 2-(tert-butyldimethylsilyloxy)ethanol. Therefore, it is necessary to establish a stable and effective analytical method for quality control of 2-(tert-butyldimethylsilyloxy)ethanol

Method used

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  • Analysis detection method of 2-(tert-butyldimethylsilyl oxyl)ethanol
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  • Analysis detection method of 2-(tert-butyldimethylsilyl oxyl)ethanol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Instruments and conditions: Waters e2695 liquid chromatography system, Waters 2489 UV / visible light detector, chromatographic column: Shimadzu Inertsil ODS-3V; C18, 4.6×250mm, 5μm, detection wavelength 205nm, column temperature 25°C, flow rate 1.0mL / min, mobile phase: A-0.01% formic acid in water, B-0.01% formic acid in acetonitrile, gradient elution settings:

[0032] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

91

9

20

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[0033] Experimental procedure: Dissolve 2-(tert-butyldimethylsilyloxy)ethanol in methanol and quantitatively dilute to make a solution containing 15 mg of 2-(tert-butyldimethylsilyloxy)ethanol per 1 mL. As the test solution, accurately measure 20 μL of the test solution and inject it into the liquid chromatograph, carry out high-performance liquid chromatography analysis according to the above conditions, and record the chromatogra...

Embodiment 2

[0036] Instruments and conditions: Waters e2695 liquid chromatography system, Waters 2489 UV / visible light detector, chromatographic column: Shimadzu Inertsil ODS-3V; C18, 4.6×250mm, 5μm, detection wavelength 205nm, column temperature 20°C, flow rate 0.7mL / min, mobile phase: A-0.01% formic acid in water, B-0.01% formic acid in acetonitrile, gradient elution settings:

[0037] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

88

12

20

12

88

30

12

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31

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12

[0038] Experimental procedure: Dissolve 2-(tert-butyldimethylsilyloxy)ethanol with acetonitrile and quantitatively dilute to make a solution containing 15 mg of 2-(tert-butyldimethylsilyloxy)ethanol per 1 mL. As the test solution, accurately measure 20 μL of the test solution and inject it into the liquid chromatograph, carry out high-performance liquid chromatography analysis according to the above conditions, and record the ...

Embodiment 3

[0041] Instruments and conditions: Waters e2695 liquid chromatography system, Waters 2489 UV / visible light detector, chromatographic column: Shimadzu Inertsil ODS-3V; C18, 4.6×250mm, 5μm, detection wavelength 205nm, column temperature 30°C, flow rate 1.2mL / min, mobile phase: A-0.01% formic acid in water, B-0.01% formic acid in acetonitrile, gradient elution settings:

[0042] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

97

3

20

3

97

30

3

97

31

97

3

40

97

3

[0043] Experimental procedure: Dissolve 2-(tert-butyldimethylsilyloxy)ethanol in methanol and quantitatively dilute to make a solution containing 15 mg of 2-(tert-butyldimethylsilyloxy)ethanol per 1 mL. As the test solution, accurately measure 20 μL of the test solution and inject it into the liquid chromatograph, carry out high-performance liquid chromatography analysis according to the above conditions, and record the chromatogra...

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Abstract

The invention relates to an analysis detection method of 2-(tert-butyldimethylsilyl oxyl)ethanol. The method is used for quality control over 2-(tert-butyldimethylsilyl oxyl)ethanol, a chromatographic column (C18, 4.6*250 mm, 5 micrometers) takes octadecylsilane chemically bonded silica as filler, a 0.01% formic acid aqueous solution serves as a mobile phase A, a 0.01% formic acid acetonitrile solution serves as a mobile phase B, gradient elution is conducted, and efficient liquid chromatography analysis detection is conducted on the condition that the detection wave length is 205 nm, and the column temperature ranges from 20 DEG C to 30 DEG C. According to the analysis detection method, 2-(tert-butyldimethylsilyl oxyl)ethanol can be effectively separated from impurities thereof, and the method has the advantagesof being high in sensitivity and degree of separation, easy to operate, good in repeatability and durability and stable and reliable in result.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography analysis method, especially an analysis and detection method for 2-(tert-butyldimethylsilyloxy)ethanol. Background technique [0002] Everolimus (everolimus) is a new generation of macrolide rapamycin derivative drugs. The drug was developed by Novartis Corp. and first launched in Germany in 2004. It is mainly used for 1) advanced renal cancer that is ineffective for other drugs; 2) it can supplement the immunosuppression of calcineurin inhibitor cyclosporine It is used to prevent the rejection of heart or kidney transplantation; 3) Drug-eluting stent drug is one of the most commonly used drugs for drug-eluting stents. [0003] 2-(tert-butyldimethylsilyloxy)ethanol is an important intermediate for the synthesis of everolimus, and its chemical formula is C 8 h 20 o 2 Si, the structural formula is as follows: [0004] [0005] Although patents WO2012103959A1 and CN101175760A descri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 张贵民魏石磊李洪伟
Owner SHANDONG NEWTIME PHARMA
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