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Method for detecting content of glycerophosphoryl choline

A technology for the content of glycerophosphocholine, which is applied in the preparation of test samples and analysis by nuclear magnetic resonance, etc., can solve the problems of many test steps, long time-consuming, complicated processing, etc., and achieve fast analysis speed, simple operation and low cost. low effect

Inactive Publication Date: 2015-09-02
SHANGHAI JIAO TONG UNIV
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Problems solved by technology

Using HPLC to determine its content, the pre-processing is complicated, and it is necessary to ensure that GPC is completely dissociated from the drug. There are many testing steps and time-consuming, and high-purity substances are required for comparison in quantification.

Method used

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  • Method for detecting content of glycerophosphoryl choline
  • Method for detecting content of glycerophosphoryl choline
  • Method for detecting content of glycerophosphoryl choline

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Embodiment 1

[0035] 2.1 Experimental conditions

[0036] set up 13 C observation frequency is 100.62MHz, spectral width is 38265.305Hz, 13 The C 90° pulse width is 3.30 μs, the proton decoupling pulse width is 100 μs, the sampling time is 0.0134 s, the relaxation delay time is 25 s, the rotational speed is 5000 Hz, and the sampling frequency is 1428 times. 13 C chemical shifts were set against the glycine carbonyl carbon signal (176.03 relative to TMS δ).

[0037] 2.2 Sample preparation of the test product

[0038] Accurately weigh the appropriate amount of GPC drug and hexamethylbenzene powder after grinding, and pass the sample through an 800 μm sieve. The portion of the sample that cannot pass through the sieve is ground again with a screw mill until all pass through an 800 μm sieve. Mix the sample thoroughly.

[0039] 2.3 Selection of internal standard and quantitative peak

[0040] When using NMR for quantification, you should first assign each carbon peak of the analyte and int...

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Abstract

The invention discloses a method for determining the content of GPC (glycerophosphoryl choline) in three types of novel medicines GPC by utilizing a solid nuclear magnetic resonance internal standard method. The method mainly comprises the following steps: adding internal standard hexamethylbenzene in a test sample, acquiring a 13C NMR spectrogram of a sample by adopting a Bruker Avance III 400MHz, a nuclear magnetic resonance spectrometer and a wideband solid CP / MAS probe, and calculating the content of GPC by the 13C peak area of the methyl group contained in the GPC and hexamethylbenzene. According to the method disclosed by the invention, the structure authentication and quantitative analysis of the GPC are completed synchronously, so that the technical problems of the content determination of three types of novel medicine GPC standard substances are solved; the method has very great significance to the GPC development of three types of novel medicines GPC and interest protection of consumers and the healthy development of the GPC medicine industry of our country, and provides reference for the subsequent research of the nuclear magnetism quantitative analysis of other medicaments.

Description

technical field [0001] The invention belongs to the technical field of development of three new drugs, Glycerophosphocholine (GPC, hereinafter referred to as GPC); in particular, it relates to a method for determining the content of GPC in GPC drugs by using a solid nuclear magnetic resonance internal standard method. Background technique [0002] With the acceleration of the world's population aging, Alzheimer's disease has become the fourth leading cause of life-threatening elderly people, seriously threatening the health and quality of life of middle-aged and elderly people. Therefore, the prevention and treatment of Alzheimer's disease has become a major topic of medical research. Glycerophosphorylcholine (GPC for short) is one of the products of phospholipid metabolism in the body, and is also the biosynthetic precursor of the important neurotransmitter acetylcholine (Acetylcholine). In vivo, the most important physiological function of GPC is to cross the blood-brain ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08G01N1/28
Inventor 代博娜吴节莉
Owner SHANGHAI JIAO TONG UNIV
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