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Method for detecting purity of distearoyl phosphatidylcholine

A technology of distearoylphosphatidylcholine and stearoylphosphatidylcholine, which is applied in the field of detection of the purity of distearoylphosphatidylcholine, can solve the problem of high experimental conditions, cumbersome processing, and Can not separate distearoylphosphatidylcholine and other problems, to solve the problem of sample purity detection and impurity control, high sensitivity and high accuracy

Pending Publication Date: 2022-07-12
JENKEM TECH CO LTD TIANJIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, NMR spectroscopy has high requirements on instruments and experimental conditions, and is not suitable for large-scale promotion.
Patent document CN101387587 discloses a method for colorimetric detection of lecithin content, but its pretreatment is cumbersome and inefficient
Patent document CN110007032A discloses a phospholipid detection method and its application. The high-performance liquid chromatography evaporative light detection method is used to detect phospholipids, but the specificity of this method is not strong, and distearoylphosphatidylcholine cannot be well separated from impurities. , so as not to meet the detection requirements for detecting the purity of distearoylphosphatidylcholine

Method used

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  • Method for detecting purity of distearoyl phosphatidylcholine
  • Method for detecting purity of distearoyl phosphatidylcholine
  • Method for detecting purity of distearoyl phosphatidylcholine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]Example 1 Optimization of chromatographic column

[0042] 1.1 Use butylsilane-bonded silica gel as filler (DAISOPAKSP-300-5-C4-BIO 4.6×250mm, 5μm, 300A) chromatographic column

[0043] The HPLC detection method specifically comprises the following steps:

[0044] (1) Chromatographic conditions:

[0045] Instrument: Shimadzu LC-16 high performance liquid chromatograph

[0046] Detector: Thermo Veo RS CAD detector

[0047] Chromatographic column: butylsilane bonded silica gel as filler (DAISOPAKSP-300-5-C4-BIO 4.6×250mm, 5μm, 300A)

[0048] Aqueous phase (mobile phase A): 0.1% aqueous trifluoroacetic acid.

[0049] Organic phase (mobile phase B): methanol to acetonitrile volume ratio 4:1 solution.

[0050] Flow rate: 1.0 mL / min.

[0051] Column temperature: 40°C.

[0052] Injection volume: 10 μL.

[0053] Workstation: Labsolution

[0054] Carry out gradient elution according to the following table:

[0055] Table 1.1. Elution procedure

[0056]

[0057] chrom...

Embodiment 2

[0091] Example 2 Optimization of Mobile Phase

[0092] 2.1, mobile phase is organic phase is methanol

[0093] The HPLC detection method specifically comprises the following steps:

[0094] (1) Chromatographic conditions:

[0095] Instrument: Shimadzu LC-16 high performance liquid chromatograph

[0096] Detector: Thermo Veo RS CAD detector

[0097] Chromatographic column: butylsilane bonded silica gel as filler (DAISOPAKSP-300-5-C4-BIO 4.6×250mm, 5μm, 300A)

[0098] Aqueous phase (mobile phase A): 0.1% aqueous trifluoroacetic acid.

[0099] Organic phase (mobile phase B): methanol.

[0100] Flow rate: 1.0 mL / min.

[0101] Column temperature: 40°C.

[0102] Injection volume: 10 μL.

[0103] Workstation: Labsolution

[0104] Carry out gradient elution according to the following table:

[0105] Table 2.1. Elution procedure

[0106]

[0107]

[0108] The result is as Figure 5 As shown, when methanol is used for the organic phase, the main peak appears late, and ...

Embodiment 3

[0110] Embodiment 3 method verification

[0111] 3.1 Solution preparation:

[0112] Blank solution: methanol, Merck, HPLC grade.

[0113] Preparation of reference stock solution: Precisely weigh 20 mg distearoyl phosphatidyl choline (DSPC), place it in a 10 mL volumetric flask, add methanol to dissolve, then add methanol to volume to the mark, shake well, and obtain 2 mg / mL reserve liquid. Accurately weigh 24 mg of distearoyl phosphatidyl choline (DSPC), put it in a 10 mL volumetric flask, add methanol to dissolve, then add methanol to make up to the mark, and shake well to obtain a 2.4 mg / mL stock solution.

[0114] Linear reference substance solution: accurately pipette 2.5mL, 1mL, 0.5mL, 0.25mL to 5mL volumetric flask of 2mg / mL reference substance stock solution respectively, add methanol to volume to the mark, shake well to obtain 1mg / mL, 0.4mg / mL , 0.2 mg / mL, 0.1 mg / mL. Accurately pipette 2.5mL of the 2.4mg / mL reference stock solution into a 5mL volumetric flask, add ...

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Abstract

The invention provides a method for detecting the purity of distearoyl phosphatidylcholine, which comprises the following steps: dissolving distearoyl phosphatidylcholine, detecting by adopting a high performance liquid chromatography, and adopting a chromatographic column taking butyl silane bonded silica gel as a stationary phase, an organic phase of a mobile phase is methanol-acetonitrile, a water phase is a trifluoroacetic acid water solution, and the volume ratio of trifluoroacetic acid to water is (0.1-0.3): 100; the method is convenient to operate and good in separation, the purity of the product is effectively controlled through a high and low concentration method, and the method meets the standards in the aspects of quantitation, linear range, repeatability, recovery rate and the like and has relatively high durability.

Description

Technical field [0001] The invention relates to the technical field of chemical analysis, specifically a method for detecting the purity of distearoylphosphatidylcholine. Background technique [0002] Phosphatidylcholine (PC), also known as lecithin or choline phospholipid, is the basic substance of life activities. It is widely present in the cell membranes and egg cells of animals, plants and humans in the form of mixtures with other phospholipid components such as phosphatidylethanolamine (PE), phosphatidic acid (PA) and inositol phospholipids (PI). Liposome is an artificial membrane in which the hydrophilic heads of phospholipid molecules are inserted into the water, and the hydrophobic tails of the liposomes extend into the air. After stirring, they form spherical liposomes with a double layer of lipid molecules. Liposome is a targeted drug carrier and a new dosage form of targeted drug delivery system. Liposomes have little toxic and side effects on the body, and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/54G01N30/64
CPCG01N30/02G01N30/06G01N30/54G01N30/64Y02P20/55
Inventor 朱丹丹李洋何平赵宣
Owner JENKEM TECH CO LTD TIANJIN
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