A method for the simultaneous quantitative determination of phospholipids and fatty acid glycerides in pharmaceutical preparations

A technology of fatty acid glycerides and pharmaceutical preparations, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of insufficient sensitivity of high-performance liquid phase analysis methods, consumption of large organic solvents such as chloroform, and non-compliance with environmental protection, etc., to avoid Effects of mutual interference and interference of other components, less amount of organic solvent, and short detection time

Active Publication Date: 2021-01-29
GUANGDONG JIABO PHARM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] When HPLC is used to analyze phospholipids, chloroform / methanol / water is often used for pretreatment. Although it can be quantitatively analyzed, the sensitivity of HPLC analysis method is not ideal, the linear range is generally narrow, and normal A large amount of organic solvents such as chloroform will be consumed during the analysis process, which does not meet the requirements of green environmental protection

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  • A method for the simultaneous quantitative determination of phospholipids and fatty acid glycerides in pharmaceutical preparations
  • A method for the simultaneous quantitative determination of phospholipids and fatty acid glycerides in pharmaceutical preparations
  • A method for the simultaneous quantitative determination of phospholipids and fatty acid glycerides in pharmaceutical preparations

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Embodiment 1

[0025] The pretreatment of embodiment one sample

[0026] Measure 1.0mL of the drug preparation sample into a 20mL headspace bottle, place it in a vacuum drying oven at 65°C and dry it under reduced pressure until dry, add 1.0mL of internal standard solution and 0.5mL of 1mol / L potassium hydroxide solution, seal it, and keep at 90°C Heat in a water bath and vibrate continuously for 10 minutes, cool to room temperature to obtain a saponified sample solution; add 10% boron trifluoride methanol solution 1mL to the saponified sample solution, seal, heat in a 90°C water bath and vibrate continuously After 5 minutes, cool to room temperature to obtain the sample solution after methyl esterification treatment; add 5 mL of n-hexane to the sample solution after methyl esterification treatment, seal, shake in a water bath at 60°C for 3 minutes, cool to room temperature, add 5 mL of saturated sodium chloride, Seal it, shake it at room temperature for 2 minutes, let it stand for stratific...

Embodiment 2

[0028] The preparation of embodiment two reference substance solution and negative solution

[0029] Take 15.00mg TA, 20.00mg DMPG and 60.00mg DSPC respectively, accurately weigh them into a 10mL volumetric flask, and dilute to volume with methanol to obtain a stock solution. Measure 1.0 mL of the stock solution in a headspace bottle, and prepare according to the method in Example 1 to obtain the reference substance solution. Take 1.0 mL of pure water in a headspace bottle and prepare according to the method in Example 1 to obtain a negative solution.

Embodiment 3

[0030] Example three detection of sample detection solution

[0031] The sample detection solution prepared in Example 1, the reference substance solution prepared in Example 2 and the negative solution are detected by gas chromatography, and the gas chromatography conditions include: the chromatographic column adopts a medium polar chromatographic column DB-WAX, and the carrier gas Helium, flow rate of 2mL / min, hydrogen flow rate of 30mL / min, air flow rate of 300mL / min, inlet temperature of 250°C, injection volume of 1μL, split injection, split ratio of 10:1, detection The detector is a hydrogen flame ionization detector, the detector temperature is 260°C, and the temperature is programmed: the initial temperature is 80°C, kept for 5 minutes, and the temperature is raised to 230°C at 50°C / min, and kept for 11 minutes. Record the chromatogram see figure 1 , the chromatographic peaks of TA, DMPG, DSPC and the internal standard in the sample detection liquid chromatogram are co...

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Abstract

The invention discloses a method for simultaneous quantitative determination of phospholipids and fatty acid glycerides in a pharmaceutical preparation. The method comprises the following steps: S1 sample pretreatment, to be more specific, performing saponification treatment and methyl esterification treatment on a pharmaceutical preparation sample; adding n-hexane in the sample after the methyl esterification treatment, performing water bath at 45-70DEG C, cooling to room temperature, adding a saturated sodium chloride solution, standing for layering, taking supernatant, and adding a desiccant for dehydrating to obtain a sample detection solution; and S2 detection of the sample detection solution, to be more specific, using a gas chromatograph to detect the sample detection solution. Themethod realizes the simultaneous quantitative determination of the phospholipids and the fatty acid glycerides in the pharmaceutical preparation, and has the advantages of high sensitivity, low detection limit, wide linear range, good accuracy, good repeatability, short detection time and less organic solvent dosage, and is in line with industrialization and green environmental protection requirements.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for simultaneously quantitatively determining phospholipids and fatty acid glycerides in drug preparations. Background technique [0002] The quantitative analysis of phospholipids and fatty acid glycerides is mostly carried out by liquid chromatography connected in series with detectors such as evaporative light scattering detector (ELSD) and charged aerosol detector (CAD), among which ELSD is the most widely used. [0003] Xu Weidong et al. published a paper titled "Determination of Phosphatidylcholine Content in Medium / Long-Chain Fat Emulsion Injection by High Performance Liquid Chromatography-Evaporative Light Scattering Detection Method" disclosed a method for detecting phosphatidylcholine by HPLC tandem ELSD. Chinese patent application CN104931618A discloses a method for multiple detection of six phospholipids in complex samples by HPLC tandem ELSD. [0004]...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/14
CPCG01N30/02G01N30/14
Inventor 李闫飞柳文俊贺周扬岳峰陈荣振徐新军
Owner GUANGDONG JIABO PHARM CO LTD
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