Separation and detection method of l-glutamic acid diethyl ester hydrochloride and its optical isomers

A technology of diethyl glutamate, optical isomers, applied in the field of analytical chemistry

Active Publication Date: 2022-03-18
YANGTZE RIVER PHARM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are no reports in the literature on the detection of its optical isomers by HPLC

Method used

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  • Separation and detection method of l-glutamic acid diethyl ester hydrochloride and its optical isomers
  • Separation and detection method of l-glutamic acid diethyl ester hydrochloride and its optical isomers
  • Separation and detection method of l-glutamic acid diethyl ester hydrochloride and its optical isomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 1.1 Chromatographic conditions

[0043] Instrument: Agilent 1260 high performance liquid chromatography;

[0044] Chromatographic column: DAICEL CROWNPAKCR-I(+), 3.0×150mm, 5μm;

[0045] Mobile phase: pH2.0 perchloric acid aqueous solution-acetonitrile (the volume ratio of perchloric acid aqueous solution to acetonitrile is 60:40);

[0046] Detection wavelength: 205nm;

[0047] Column temperature: 25°C;

[0048] Injection volume: 20μl;

[0049] Flow rate: 1.0ml / min;

[0050] Running time: 20min.

[0051] 1.2 Sample preparation

[0052] Blank solution: water.

[0053] Need testing solution: Take about 60mg of L-diethyl glutamate hydrochloride, accurately weigh it, put it in a 10ml measuring bottle, add water to dissolve and dilute to the mark, shake well, and use it as the need testing solution.

[0054] Control solution: Accurately measure 1ml of the test solution, put it in a 200ml measuring bottle, dilute with water to the mark, shake well, and use it as a con...

Embodiment 2

[0063] 2.1 Chromatographic conditions

[0064] Instrument: Agilent 1260 high performance liquid chromatography;

[0065] Chromatographic column: DAICEL CROWNPAKCR-I(+), 3.0×150mm, 5μm;

[0066] Mobile phase: pH2.0 perchloric acid aqueous solution-acetonitrile (the volume ratio of perchloric acid aqueous solution to acetonitrile is 60:40);

[0067] Detection wavelength: 205nm;

[0068] Column temperature: 25°C;

[0069] Injection volume: 20μl;

[0070] Flow rate: 0.8ml / min;

[0071] Running time: 20min.

[0072] 2.2 Sample preparation

[0073] Same as Example 1

[0074] 2.3 Determination

[0075] Take 20 μl of the resolution solution and inject it into a high-performance liquid chromatograph, record the chromatogram, the peaks of optical isomers and L-diethyl glutamate hydrochloride appear sequentially, and the resolution should be greater than 1.5.

[0076] Take the test solution and 20 μl of the control solution respectively and inject them into the high-performance li...

Embodiment 3

[0079] 3.1 Chromatographic conditions

[0080] Instrument: Agilent 1260 high performance liquid chromatography;

[0081] Chromatographic column: DAICEL CROWNPAKCR-I(+), 3.0×150mm, 5μm;

[0082] Mobile phase: pH2.0 perchloric acid aqueous solution-acetonitrile (the volume ratio of perchloric acid aqueous solution to acetonitrile is 60:40);

[0083] Detection wavelength: 205nm;

[0084] Column temperature: 25°C;

[0085] Injection volume: 20μl;

[0086] Flow rate: 1.2ml / min;

[0087] Running time: 20min.

[0088] 3.2 Sample preparation

[0089] Same as Example 1

[0090] 3.3 Determination

[0091] Take 20 μl of the resolution solution and inject it into the high-performance liquid chromatograph, and record the chromatogram. Optical isomers and L-glutamic acid diethyl ester hydrochloride elute in sequence, and the resolution should be greater than 1.5.

[0092] Take the test solution and 20 μl of the control solution respectively and inject them into the high-performanc...

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Abstract

The invention discloses a separation and detection method of L-glutamic acid diethyl ester hydrochloride and its optical isomers. The separation and detection method adopts high performance liquid chromatography, the stationary phase is a silica gel chiral column, and the mobile phase is Reverse phase solvent: Perchloric acid in water - acetonitrile. The method of the invention has the characteristics of good separation, high sensitivity, strong specificity, etc., and can quickly and accurately perform quality control on L-diethyl glutamate hydrochloride.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and detecting L-glutamic acid diethyl ester hydrochloride and its optical isomers. Background technique [0002] Diethyl L-glutamate hydrochloride is an important pharmaceutical and chemical raw material, which can be used to produce raltitrexed, pemetrexed and other drugs. Its chemical structure is as follows: [0003] [0004] There will be a certain amount of optical isomers in L-diethyl glutamate hydrochloride, namely D-diethyl glutamate hydrochloride, its chemical structure is as follows: [0005] [0006] The optical isomer may remain in the drug through subsequent reactions, affecting the quality of the drug. Therefore, it is necessary to carry out quality control on the optical isomer impurities in L-diethyl glutamate hydrochloride. Controlling the content of optical isomers in L-diethyl glutamate hydrochloride is of great si...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 韩林徐浩宇董达文蔡伟徐瑛宣景安吴青青李博于向东夏雨王莲莲
Owner YANGTZE RIVER PHARM GRP CO LTD
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