Method for detecting residual solvents in heparin sodium by headspace gas chromatography

A technology of headspace gas chromatography and residual solvents, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of poor applicability, achieve high sensitivity, high separation, and overcome the effects of poor system applicability

Inactive Publication Date: 2018-07-24
HUBEI YINUORUI BIOLOGICAL PHARMA
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0007] In order to overcome the above-mentioned deficiencies of the prior art, the present invention provides a method for detecting residual solvents in heparin sodium by headspace gas chromatography. The sample equilibration temperature overcomes the technical problem of poor system applicability of the existing detection method, so that the relative standard deviation of the peak area ratio of the analyte to the internal standard is less than 1.0% when the reference substance is repeatedly injected, and the system applicability meets the requirements

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  • Method for detecting residual solvents in heparin sodium by headspace gas chromatography
  • Method for detecting residual solvents in heparin sodium by headspace gas chromatography
  • Method for detecting residual solvents in heparin sodium by headspace gas chromatography

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Embodiment 1

[0069] The invention provides a method for detecting residual solvents in heparin sodium by headspace gas chromatography, the method comprising the following steps:

[0070] 1. Prepare the solution

[0071] (1) Preparation of internal standard solution: add 150ml of ultrapure water to a 250ml volumetric flask, then precisely weigh 25μl of n-propanol (density 0.80g / ml) into the 250ml volumetric flask, dilute with water to the mark, and shake well to prepare 80μg / ml n-propanol solution;

[0072] (2) Preparation of the test solution: Accurately weigh 2.0g of heparin sodium sample into a 10ml volumetric flask, add internal standard solution to dissolve and dilute to the mark, shake well; accurately pipette 3.0ml of the solution, place In the headspace bottle of sodium chloride 500mg, seal, be mixed with need testing solution; Repeat preparation 2 parts, as need testing solution 1, need testing solution 2.

[0073] (3) Preparation of mixed reference substance stock solution: add ...

Embodiment 2

[0101] Embodiment 2: specificity experiment

[0102] 1. Solution preparation

[0103] Blank solution: Accurately measure 3.0ml of water, put it in a headspace bottle pre-added with 500mg of sodium chloride, and seal it.

[0104] Preparation of internal standard solution: Add 150ml of ultrapure water into a 250ml volumetric flask, then precisely weigh 25μl of n-propanol (density 0.80g / ml) into the 250ml volumetric flask, dilute to the mark with water, shake well to prepare 80μg / ml n-propanol solution;

[0105] n-propanol reference substance solution: Accurately measure 3.0ml of internal standard solution, put it in a headspace bottle pre-added with 500mg of sodium chloride, and seal it.

[0106] Methanol reference substance solution: Accurately weigh 0.04g of methanol, put it into a 100ml volumetric flask with about 30ml of water, add water to dilute to the mark, shake well, take 3.0ml of this solution, put it into a headspace bottle with 500mg of sodium chloride added in adv...

Embodiment 3

[0117] Embodiment 3: System suitability experiment

[0118] Get first 5 parts of mixed reference substance parallel samples in embodiment 1, each parallel sample injection needle carries out gas phase detection, record chromatogram, chromatogram is as follows Figure 9-13 shown. The data reflected in the chromatogram were sorted out and analyzed, and the analysis results of the system suitability test results are shown in Table 1.

[0119] Table 2 Results of solvent residual system suitability test (headspace equilibrium temperature 80°C)

[0120]

[0121]

[0122] As can be seen from the test results, each analyte is well separated under the gas chromatographic conditions established by the technical scheme of the present invention, the column efficiency meets the requirements, the RSD value of the peak area ratio repeatability of each analyte is less than 5.0%, and the method system applicability meets the requirements.

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Abstract

The invention relates to the technical field of solvent residual detection of drugs, and concretely relates to a method for detecting residual solvents in heparin sodium by headspace gas chromatography. The method optimizes the headspace sampling balance temperature which is an important parameter affecting the peak area ratio of the analytes to an internal standard by adopting the headspace gas chromatography against the technical problem of poor system adaptability of methods for detecting the residual solvents in the heparin sodium in the prior art, and the headspace balance temperature isoptimized to 78-82 DEG C from 90 DEG C. The method for detecting residual solvents in heparin sodium by headspace gas chromatography allows the relative standard deviation of the peak area ratio of the analytes to the internal standard during the repeated introduction of a control to be less than 1.0% and the system applicability to meet requirements, has the advantages of good specificity, good resolution of the analytes, good repeatability and high sensitivity, the detection limit of methanol is 0.0008%, the detection limit of ethanol is 0.0002%, the detection limit of acetone is 0.0001%, the quantitation limit of methanol is 0.0023%, the quantitation limit of ethanol is 0.0007%, and the quantitation limit of acetone is 0.0003%.

Description

technical field [0001] The invention relates to the technical field of detection of drug solvent residues, in particular to a method for detecting residual solvents in heparin sodium by headspace gas chromatography. Background technique [0002] Heparin sodium is a mucopolysaccharide sulfate anticoagulant. Heparin sodium is the sodium salt of aminodextran sulfate extracted from the intestinal mucosa of pigs or cattle, and belongs to mucopolysaccharides. Studies in recent years have proved that heparin sodium also has the effect of lowering blood lipids. Heparin is the compound with the most complex molecular structure known in the world so far, and it cannot be artificially chemically synthesized in the short term. Currently, only heparin derived from pig small intestinal mucosa can be used for clinical treatment. The raw material of heparin API is crude heparin, which can only be extracted from the small intestinal mucosa of healthy pigs. Because it contains a large amoun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/30
Inventor 罗锡川王晶晶
Owner HUBEI YINUORUI BIOLOGICAL PHARMA
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