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Method for analyzing residual solvent in enoxaparin sodium

A technology for enoxaparin sodium and residual solvents, which is applied in the field of analytical chemistry, can solve errors, cannot accurately analyze the residual levels of methanol, ethanol and dichloromethane in enoxaparin sodium, and qualitatively identify residual organic solvents in enoxaparin sodium and long quantitative analysis process

Inactive Publication Date: 2020-06-16
HUBEI YINUORUI BIOLOGICAL PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides a residual solvent analysis method in enoxaparin sodium, which solves the problem that the existing residual solvent analysis method cannot accurately analyze the residual amount of methanol, ethanol and dichloromethane in enoxaparin sodium In addition, the process of qualitative and quantitative analysis of organic solvent residues in enoxaparin sodium is relatively long, and there are certain errors

Method used

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  • Method for analyzing residual solvent in enoxaparin sodium
  • Method for analyzing residual solvent in enoxaparin sodium
  • Method for analyzing residual solvent in enoxaparin sodium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Limits of detection and quantitation:

[0046] 1. Solution Preparation

[0047] 50% dimethyl sulfoxide stock solution: take 300 ml of water and 300 ml of dimethyl sulfoxide, put them in a 1000 ml beaker, stir well, and cool to room temperature.

[0048] Internal standard solution: take 50 μl of n-propanol, put it in a 500ml volumetric flask containing about 200ml of 50% dimethyl sulfoxide solution, add 50% dimethyl sulfoxide solution to dilute to the mark, and shake well to obtain 80 μg / ml of n-propanol solution.

[0049] Blank solution: Pipette 5.0ml of internal standard solution precisely, place it in a 20ml headspace bottle, and seal it.

[0050] Methanol control stock solution: Take about 0.3g of methanol, weigh it accurately, put it into a 50ml volumetric flask containing about 20ml of internal standard solution, dilute the internal standard solution to the mark, and shake well.

[0051] Ethanol control stock solution: Take about 0.5g of ethanol, weigh it accura...

Embodiment 2

[0071] Accuracy experiment:

[0072] 1. Solution Preparation

[0073] 50% dimethyl sulfoxide solution: take 600 ml of water and 600 ml of dimethyl sulfoxide, put them in a 2000 ml beaker, stir evenly, and cool to room temperature.

[0074] Internal standard solution: take 100 μl of n-propanol, put it in a 1000ml volumetric flask of about 500ml 50% dimethyl sulfoxide solution, add 50% dimethyl sulfoxide solution to dilute to the mark, shake well to get 80 μg / ml n-propanol solution.

[0075] Blank solution: Pipette 5.0ml of internal standard solution precisely, place it in a 20ml headspace bottle, and seal it.

[0076] Stock solution 1: Take about 0.3g of methanol, weigh it accurately, put it into a 50ml volumetric flask containing about 20ml of internal standard solution, add internal standard solution to dilute to the mark, and shake well.

[0077] Stock solution 2: Take about 0.5g of ethanol, weigh it accurately, put it into a 50ml volumetric flask containing about 20ml of...

Embodiment 3

[0089] Durability test:

[0090] When evaluating small changes in the parameters of the determination conditions by changing the headspace temperature, different flow rates, different column temperatures, and different chromatographic columns, the system applicability should meet the following requirements:

[0091] The degree of separation between each peak in the control solution should be greater than 1.5; the number of theoretical plates of methanol, ethanol, dichloromethane, and n-propanol peaks in the control solution should not be less than 5000; Chloromethane and the relative standard deviation of the internal standard peak area ratio are all no more than 5.0%; The relative standard deviations of the peak area ratios of n-propanol were not more than 5.0%.

[0092]

[0093] 1. Solution Preparation

[0094] 50% dimethyl sulfoxide solution: take 300 ml each of water and dimethyl sulfoxide, put them in a 1000 ml beaker, stir evenly, and cool to room temperature.

[0...

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Abstract

The invention discloses a method for analyzing a residual solvent in enoxaparin sodium. The method specifically comprises the following steps: S1, taking a capillary column, setting carrier gas of thecapillary column to be nitrogen, setting the column flow rate of the capillary column to be 3.0 ml / min, the hydrogen flow rate to be 35.0 ml / min, the air flow to be 350.0 ml / min, the tail blowing flow to be 30ml / min, the column temperature of the capillary column to be 120 DEG C, the temperature of a sample inlet to be 200 DEG C, and the split ratio to be 20: 1, using a hydrogen flame ionizationdetector as detection equipment, and setting the temperature of the detector to be 250 DEG C; and S2, carrying out sample introduction of a sample solution in a headspace sample introduction mode, andsetting the equilibrium temperature of a headspace sample injector to be 85 DEG C. The invention relates to the technical field of analytical chemistry. According to the method for analyzing the residual solvent in the enoxaparin sodium, a simple gas chromatography determination method is adopted, the residual quantity level of methanol, ethanol and dichloromethane in the enoxaparin sodium is accurately analyzed, and qualitative and quantitative analysis can be more rapidly and accurately carried out on organic solvent residues in the enoxaparin sodium.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for analyzing residual solvents in enoxaparin sodium. Background technique [0002] Preparation of enoxaparin sodium - Methanol, ethanol and methylene chloride are used in the synthesis of heparin benzyl ester. If the residual amount of organic solvent in the drug exceeds a certain limit, it will be harmful to the human body. The limits of organic solvents are stipulated, methanol, ethanol and dichloromethane are 0.3%, 0.5%, and 0.06% respectively, so the analysis and detection of residual solvents is of great significance to the safe use of enoxaparin sodium, so it is necessary to The level of residual organic solvents in noparin sodium was effectively confirmed. [0003] At present, headspace gas chromatography is used to detect the residual organic solvents in enoxaparin sodium raw materials by headspace gas chromatography, but the existing residual solv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/68
CPCG01N30/06G01N30/68
Inventor 罗锡川何锐李晶
Owner HUBEI YINUORUI BIOLOGICAL PHARMA
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