Analysis method of methylprednisolone intermediate

A technology of methylprednisolone and an analytical method is applied in the field of detection and analysis of methylprednisolone intermediates and achieves the effects of strong specificity, good separation and high sensitivity

Pending Publication Date: 2022-03-15
武汉九珑人福药业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no analytical method for methylprednisolone iodide intermediates reported in the literature

Method used

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  • Analysis method of methylprednisolone intermediate
  • Analysis method of methylprednisolone intermediate
  • Analysis method of methylprednisolone intermediate

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0039] Preparation example 1: preparation of the sample to be tested

[0040] Add 0.1g of calcium chloride and 10mL of methanol into a 25ml single-necked bottle, dissolve and add 1.7g of iodine, and use it as iodine solution for later use. Add 2g of ammonium chloride and 10mL of water into a 25ml single-necked bottle to prepare an ammonium chloride solution, which will be used as an ammonium chloride solution for later use. Add 20mL of dichloromethane, 0.2g of calcium chloride, 0.3g of calcium oxide, 2g of methylprednisolone dehydrogenate and 10mL of methanol into a 100ml three-neck flask, add iodine solution dropwise, and react for about 1 hour. Pump the prepared ammonium chloride solution into the three-necked flask, and react for about 2 hours; add 30 mL of water to the reaction solution under stirring, filter, wash with a small amount of water, and collect the filter cake to obtain methylprednisolone iodide.

Embodiment 1

[0042] Chromatographic conditions:

[0043] Injection volume: 20μl, detection wavelength: 230nm, chromatographic column: octadecylsilane bonded silica gel as filler (YMC, ODS-A, 15cm*4.6mm, 5μm), flow rate: 1ml / min, column Temperature: 20°C, mobile phase: methanol, water and trifluoroacetic acid, the volume ratio is 62:38:0.01, sample configuration: take an appropriate amount of the sample to be tested, weigh it accurately, dissolve it with an appropriate amount of methanol, and dilute it with the mobile phase to 0.4mg / ml concentration of the solution, shake well, accurately measure 20μl into the liquid chromatograph, record the chromatogram to 1.5 times the retention time of the main peak, the results are shown below.

[0044]

[0045] Remarks: Impurity A is methylprednisolone, impurity B is methylprednisolone dehydrogenate, impurity C is an unknown impurity with RRT ≈ 0.94, and impurity D is an unknown impurity with RRT ≈ 1.59.

Embodiment 2

[0047] Chromatographic conditions:

[0048] Injection volume: 20μl, detection wavelength: 240nm, chromatographic column: octadecylsilane bonded silica gel as filler (YMC, ODS-A, 15cm*4.6mm, 5μm), flow rate: 1ml / min, column Temperature: 30°C, mobile phase: methanol, water and trifluoroacetic acid, the volume ratio is 62:38:0.01, sample configuration: take an appropriate amount of the sample to be tested, weigh it accurately, dissolve it with an appropriate amount of methanol, and dilute it with the mobile phase to 0.5mg / ml concentration of the solution, shake well, accurately measure 20μl into the liquid chromatograph, record the chromatogram to twice the retention time of the main peak, the results are shown below.

[0049]

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Abstract

The invention discloses an analysis method of a methylprednisolone intermediate, which is characterized in that a high performance liquid chromatography method is adopted, and a substance to be detected is eluted. Chromatographic conditions are as follows: a stationary phase is a chromatographic column of octadecylsilane chemically bonded silica, in mobile phases, a mobile phase A is water, and a mobile phase B is methanol; the volume ratio of the water to the methanol is (50: 50)-(67: 33); the substance to be detected comprises methylprednisolone-iodide and / or methylprednisolone-diiodide. The analysis method provided by the invention has the characteristics of good separation degree, simplicity, rapidness, strong specificity, high sensitivity and the like.

Description

technical field [0001] The invention relates to the field of medical detection and analysis, in particular to a detection and analysis method for methylprednisolone intermediates. Background technique [0002] Methylprednisolone is 11β,17,21-trihydroxy-6α-methylpregna-1,4-diene-3,20-dione, which is a synthetic glucocorticoid and belongs to the middle-effect glucocorticoid , has anti-inflammatory, immune mechanism and anti-allergic effects. Methylprednisolone can inhibit the proliferation of connective tissue, reduce the permeability of capillary wall and cell membrane, reduce inflammatory exudation, and inhibit the formation and release of histamine and other toxic substances. Its water and sodium retention and potassium excretion effects are smaller than those of prednisone. It has stronger anti-inflammatory and anti-allergic effects and fewer side effects. It is mainly used for allergic and inflammatory diseases and organ transplantation to prevent rejection. It can also ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8809
Inventor 李淑云刘诚符洁李洁余丽黄文莲汪洋周凯黄恋清王晓宇邓娟
Owner 武汉九珑人福药业有限责任公司
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