A kind of high performance liquid phase detection method of glycyl-d-glutamine

A glutamine and high-performance liquid phase technology, applied in the field of high-performance liquid chromatography detection, can solve the problems of difficult separation, long reaction time, cumbersome operation steps, etc.

Active Publication Date: 2021-07-06
SHANDONG WEIGAO PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] When developing a drug with an asymmetric center, it is necessary to use a variety of chiral chromatographic columns and chiral mobile phases for testing, which takes a long time to test and the effect is not ideal
Glycylglutamine is the terminal absorption, and the ultraviolet absorption is not strong. The separation and determination of glycylglutamine isomers using chiral chromatographic columns is not only costly, but also difficult to separate.
In the prior art, other products with weaker ultraviolet absorption have been reported to be derivatized by derivatization reagents and then separated by ordinary chromatographic columns. However, the method requires a long reaction time and requires steps such as solvent drying, redissolution, and filtration. , the operation steps are cumbersome

Method used

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  • A kind of high performance liquid phase detection method of glycyl-d-glutamine
  • A kind of high performance liquid phase detection method of glycyl-d-glutamine
  • A kind of high performance liquid phase detection method of glycyl-d-glutamine

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Experimental program
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Effect test

Embodiment 1

[0050] Chromatographic conditions: covalently bonded on the surface of silica gel-quinine (8R, 9S)-(1R, 2R)-cyclohexylsulfamic acid derivatives as a chromatographic column, mobile phase is formic acid-diethylamine-methanol ( 1.9:2.6:995.5), the detection wavelength is 248nm, the flow rate is 0.2ml / min, the column temperature is 20°C, and the injection volume is 2μl.

[0051]Preparation of the test solution: Accurately weigh an appropriate amount of glycyl-L-glutamine, dilute it with water to a solution containing 3mg of glycyl-L-glutamine per 1ml of water, as the test solution; Take appropriate amount of glycyl-L-glutamine and glycyl-D-glutamine, dilute with water so that every 1ml of water contains 3mg of glycyl-L-glutamine, glycyl-D-glutamine 4.5 μg of the mixed solution, as a mixed reference solution. Precisely measure 10 μl of the test solution, put it in a dry derivation tube (diameter 6 mm, height 50 mm), add 30 μl of buffer solution (Buffer1), vortex mix, add 60 μl of ...

Embodiment 2

[0054] Chromatographic conditions: covalently bonded on the surface of silica gel-quinine (8R, 9S)-(1R, 2R)-cyclohexylsulfamic acid derivatives as a chromatographic column, mobile phase is formic acid-diethylamine-methanol ( 1.9:2.6:995.5), the detection wavelength is 248nm, the flow rate is 0.2ml / min, the column temperature is 22°C, and the injection volume is 2μl.

[0055] Preparation of the test solution: Accurately weigh an appropriate amount of glycyl-L-glutamine, dilute it with water to a solution containing 3mg of glycyl-L-glutamine per 1ml of water, as the test solution; Take appropriate amount of glycyl-L-glutamine and glycyl-D-glutamine, dilute with water so that every 1ml of water contains 3mg of glycyl-L-glutamine, glycyl-D-glutamine 4.5 μg of the mixed solution, as a mixed reference solution. Precisely measure 10 μl of the test solution, put it in a dry derivation tube (diameter 6 mm, height 50 mm), add 30 μl of buffer solution (Buffer1), vortex mix, add 60 μl of...

Embodiment 3

[0058] Chromatographic conditions: covalently bonded on the surface of silica gel-quinine (8R, 9S)-(1R, 2R)-cyclohexylsulfamic acid derivatives as a chromatographic column, mobile phase is formic acid-diethylamine-methanol ( 1.9:2.6:995.5), the detection wavelength is 248nm, the flow rate is 0.22ml / min, the column temperature is 20°C, and the injection volume is 2μl.

[0059] Preparation of the test solution: Accurately weigh an appropriate amount of glycyl-L-glutamine, dilute it with water to a solution containing 3mg of glycyl-L-glutamine per 1ml of water, as the test solution; Take appropriate amount of glycyl-L-glutamine and glycyl-D-glutamine, dilute with water so that every 1ml of water contains 3mg of glycyl-L-glutamine, glycyl-D-glutamine 4.5 μg of the mixed solution, as a mixed reference solution. Precisely measure 10 μl of the test solution, put it in a dry derivation tube (diameter 6 mm, height 50 mm), add 30 μl of buffer solution (Buffer1), vortex mix, add 60 μl o...

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Abstract

The invention discloses a high-efficiency liquid-phase detection method for glycyl-D-glutamine, comprising the following steps: preparing a test solution; preparing a mixed reference solution; deriving the test solution; and deriving the mixed reference solution; Chromatography: Precisely measure 2 μl of each sample derived from step (3) and step (4). After the chiral chromatographic column is well balanced, inject it into the liquid chromatograph, collect the chiral separation chromatogram, record the chromatogram for 60 minutes, and check seperate effect. The present invention realizes the problem of chiral separation of glycyl-L-glutamine and glycyl-D-glutamine, improves the test efficiency, and the stability of the chiral column is relatively good. Good separation effect, wide application range and good economic value.

Description

technical field [0001] The invention belongs to the technical field of high performance liquid chromatography detection and relates to a high performance liquid phase detection method of glycyl-D-glutamine. Background technique [0002] The presence of amino acids in the human body not only provides important raw materials for protein synthesis, but also provides a material basis for promoting growth, normal metabolism, and maintaining life. Amino acid drugs have low side effects, high drug efficacy, strong pertinence, and will not accumulate in the body to cause poisoning. [0003] Glycyl-L-glutamine is often used to provide glutamine to promote protein synthesis. The amino acids that make up proteins are all L-type amino acids, and the drugs obtained through chemical synthesis are often enantiomers, not a single optical Isomers, in many cases, there are significant differences in the pharmacological activity, metabolic process, metabolic rate and toxicity of a pair of ena...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/067G01N2030/884
Inventor 杨万运王智军冷嘉琦罗艳玲韩瑞花姜吉慧
Owner SHANDONG WEIGAO PHARM CO LTD
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