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Methyl 3-(2-(2-hydroxyethoxy)ethoxy)propanoate modification agent detection method

A technology of methyl diethylene glycol propionate and a detection method, applied in the detection field

Inactive Publication Date: 2015-05-13
宁波北仑大港科技创新服务中心有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] This modifier is widely used in the modification research and application of various drugs, and there is no report on the detection and analysis of polyethylene glycol modifier at home and abroad.

Method used

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  • Methyl 3-(2-(2-hydroxyethoxy)ethoxy)propanoate modification agent detection method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Preparation of methyl diethylene glycol propionate: Add diethylene glycol and methyl acrylate to ether, first ultrasonically vibrate for half an hour, then add catalyst nano-gold, ultrasonic power is 65-85kw, then continue to vibrate for 1.5 hours, under pressure 0.1Mpa, the reaction temperature is 10°C to start the reaction, and the reaction time is 5 hours. Wherein, the consumption of nano-gold is 0.5% of the total mass of diethylene glycol and methyl acrylate, the consumption of ether is 10% of the total mass of diethylene glycol and methyl acrylate, and the mass ratio of diethylene glycol to methyl acrylate 1:1.

[0023] Diethylene glycol propionate methyl esterification modifier detection:

[0024] a) Preparation of standard stock solution: Weigh 100mg of methyl diethylene glycol propionate, dissolve in water and set the volume to 1000mL to obtain standard stock solution, and store at 4°C;

[0025] b) Preparation of standard solution: pipette 1, 2, 3, 4 and 5mL o...

Embodiment 2

[0029] Preparation of methyl diethylene glycol propionate: Add diethylene glycol and methyl acrylate to ethanol, first ultrasonically vibrate for half an hour, then add catalyst nano-silver, ultrasonic power is 65-85kw, then continue to vibrate for half an hour, under pressure 0.5Mpa, the reaction temperature is 180°C to start the reaction, and the reaction time is 8 hours. Wherein, the consumption of nano-silver is 0.8% of the total mass of diethylene glycol and methyl acrylate, the consumption of ethanol is 15% of the total mass of diethylene glycol and methyl acrylate, the mass ratio of diethylene glycol and methyl acrylate It is 1:1.2.

[0030] Diethylene glycol propionate methyl esterification modifier detection:

[0031] a) Preparation of standard stock solution: Weigh 100mg of methyl diethylene glycol propionate, dissolve in water and set the volume to 1000mL to obtain standard stock solution, and store at 4°C;

[0032] b) Preparation of standard solution: pipette 1, ...

Embodiment 3

[0036] Preparation of methyl diethylene glycol propionate: Add diethylene glycol and methyl acrylate to acetonitrile, first vibrate ultrasonically for half an hour, then add catalyst cerium oxide and nano-magnesium oxide, the ultrasonic power is 65-85kw, and then continue to vibrate for 2.5 Hours, the reaction was started at a pressure of 0.8Mpa and a reaction temperature of 220° C., and the reaction time was 10 hours. Wherein, the consumption of cerium oxide and nano magnesium oxide is 1.1% of the total mass of diethylene glycol and methyl acrylate, cerium oxide and nano magnesium oxide each account for half, and the consumption of acetonitrile is 1.1% of the total mass of diethylene glycol and methyl acrylate. 20%, the mass ratio of diethylene glycol to methyl acrylate is 1:1.85.

[0037] Diethylene glycol propionate methyl esterification modifier detection:

[0038] a) Preparation of standard stock solution: Weigh 100mg of methyl diethylene glycol propionate, dissolve in w...

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Abstract

The invention relates to a methyl 3-(2-(2-hydroxyethoxy)ethoxy)propanoate modification agent detection method. The detection method comprises the following steps: preparing a standard sample; preparing a standard liquid; drawing a standard curve; and determining, namely, injecting a to-be detected sample solution into ion extrusion high performance liquid chromatography for detection, referencing the standard curve and performing peak area quantitative calculation according to quantitative ion. The detection method is rapid, simple, accurate, mild in conditions and easy to operate, is applicable to PEG microscale and semi-microscale determination, and is applicable to PEG modification agents and content determination and quality control of PEG modified medicaments.

Description

technical field [0001] The invention relates to a detection method, in particular to a fast, simple and accurate detection method of diethylene glycol propionate methyl esterification modifier. Background technique [0002] Polyethylene glycol (PEG) is the polymer with the lowest level of protein and cell absorption among known polymers so far. Due to the non-toxicity and good biocompatibility of PEG, the PEG modification of drugs is to couple the activated PEG chemically. The process of linking to the drug, after PEGylation, can improve the physical and chemical properties and biological activity of the drug, improve the properties of pharmacokinetics and pharmacodynamics, significantly enhance the solubility and stability of the drug, reduce immunogenicity and antigenicity, It reduces toxic and side effects and increases biological activity and curative effect in vivo. This technology has now been applied to proteins (peptides), enzymes, antibodies and small molecule drugs...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 施立钦邱从平华旭
Owner 宁波北仑大港科技创新服务中心有限责任公司
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