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A kind of high performance liquid chromatography analysis method of sirolimus

A high-performance liquid chromatography and analytical method technology, applied in the field of pharmaceutical analysis, can solve the problems of poor stability of experimental results and large data deviation, and achieve the effect of good stability and strong data reproducibility

Active Publication Date: 2017-01-18
WUXI FORTUNE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing technology, isocratic is usually used to solve the content problem, and the gradient is used to solve the impurity problem, but due to the sharp change of the gradient, the stability of the experimental results is often poor, and the data deviation is large

Method used

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  • A kind of high performance liquid chromatography analysis method of sirolimus
  • A kind of high performance liquid chromatography analysis method of sirolimus
  • A kind of high performance liquid chromatography analysis method of sirolimus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Determination of content and impurities of sirolimus API.

[0027] High performance liquid chromatography conditions:

[0028] Chromatographic column: Zorbax Eclipse plus C18, size 4.6mm×150mm, 3μm;

[0029] Mobile phase ratio is: mobile phase A: mobile phase B = 20:80 (volume ratio), mobile phase A is composed of phosphoric acid: sodium heptanesulfonate: water = 0.1:0.01:1 (mass ratio), mobile phase Consists of methanol: acetonitrile=15:85 (volume ratio) in B;

[0030] The detection wavelength is 277nm;

[0031] The flow rate is 1.5ml / min;

[0032] Column temperature 30°C;

[0033] Injection volume 20μL;

[0034] Diluent: 0.1% phosphoric acid solution: acetonitrile = 50:70 (volume ratio).

[0035] Experimental steps:

[0036] Solution preparation:

[0037] Get about 25mg of sirolimus bulk drug, accurately weighed, place in a 25ml volumetric flask, add an appropriate amount of diluent to dissolve and dilute to the mark, shake well, as the test solution; accurate...

Embodiment 2

[0044] Determination of content and impurities in sirolimus tablets.

[0045] High performance liquid chromatography conditions:

[0046] Chromatographic column: Shimadzu Inertsil C18, size 4.6mm×150mm, 3μm;

[0047] Mobile phase ratio is: mobile phase A: mobile phase B = 18:82 (volume ratio), mobile phase A is composed of phosphoric acid: sodium heptanesulfonate: water = 0.1:0.01:1 (mass ratio), mobile phase B is made up of methanol: acetonitrile=15:85 (volume ratio);

[0048] The detection wavelength is 277nm;

[0049] The flow rate is 1.6ml / min;

[0050] Column temperature 25°C;

[0051] The injection volume was 20 μL.

[0052] Diluent: 0.1% phosphoric acid solution: acetonitrile = 50:75 (volume ratio).

[0053] Experimental steps:

[0054] Solution preparation:

[0055] Take an appropriate amount of sirolimus tablet (approximately equivalent to 25 mg sirolimus), weigh it accurately, place it in a 25ml volumetric flask, add an appropriate amount of diluent to dilute...

Embodiment 3

[0062] Determination of content and impurities in sirolimus capsules.

[0063] High performance liquid chromatography conditions:

[0064] Chromatographic column: Dima II C18, the size is 4.6mm×150mm, 3μm;

[0065] Mobile phase ratio is: mobile phase A: mobile phase B = 22:78 (volume ratio), mobile phase A is composed of phosphoric acid: sodium heptanesulfonate: water = 0.1:0.01:1 (mass ratio), mobile phase B is made up of methanol: acetonitrile=15:85 (volume ratio);

[0066] The detection wavelength is 277nm;

[0067] The flow rate is 1.8ml / min;

[0068] Column temperature 28°C;

[0069] The injection volume was 20 μL.

[0070] Diluent: 0.1% phosphoric acid solution: acetonitrile = 50:65 (volume ratio).

[0071] Experimental steps:

[0072] Solution preparation:

[0073] Take an appropriate amount of sirolimus capsule content (approximately equivalent to 25 mg sirolimus), weigh it accurately, place it in a 25ml volumetric flask, add an appropriate amount of diluent to...

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Abstract

The invention provides a high performance liquid chromatography analysis method of sirolimus. A sample solution containing the sirolimus is led into a chromatographic column, quantitative analysis is performed by adopting a reverse liquid chromatography external-reference percentage method, and the liquid chromatography conditions are as follows: the chromatographic column uses octadecyl silane bonded silica gel as a filling material, and the specifications are 4.6 mm * 150 mm and 3 microns; a mobile phase is the mixed solution of a mobile phase A and a mobile phase B with the volume ratio of 18:82-22:78 and is used for isocratic elution, the mass ratio of the phosphoric acid to sodium heptanesulfonate to water in the mobile phase A is 0.1:0.01:1, and the volume ratio of methanol to acetonitrile in the mobile phase B is 15:85; the detection wavelength is 270-280 nm; the flow velocity is 1.5-2.0 ml / min; the temperature of the column is 25-35 DEG C; the sample injection volume is 15-30 microliters. The high performance liquid chromatography analysis method has the advantages of being practical, reliable, better in stability and good in data reproducibility and can separate out impurities RRT1.07, C and RRT1.14.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to a high-performance liquid chromatography analysis method for sirolimus. Background technique [0002] Sirolimus, also known as rapamycin, is a macrolide antibiotic immunosuppressant. In 1977, sirolimus was found to have an immunosuppressive effect, and in 1989, sirolimus was used as a new drug for the treatment of organ transplant rejection. After Phase III clinical trials, sirolimus oral solution developed by Wyeth Pharmaceuticals was first launched in the United States in October 1999, and FDA allowed it to be used as a drug with high safety in the clinical prevention and treatment of renal transplant rejection. [0003] In order to ensure the quality of the subsequent research and development and production of sirolimus, it is necessary to control the quality of the API and its preparations. Therefore, it is particularly urgent for pharmaceutical manufactur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 张莹史佳栋付静游云龙成梁曹峥赵文俊杨亮
Owner WUXI FORTUNE PHARMA