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Analysis and detection method of L-diethyl glutamate

A technology of diethyl glutamate and a detection method, which is applied in the field of high performance liquid chromatography analysis, can solve problems affecting the quality of the final product, and achieve the effects of stable and reliable results, good repeatability and durability, and quality assurance

Inactive Publication Date: 2015-04-15
SHANDONG NEWTIME PHARMA
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AI Technical Summary

Problems solved by technology

[0005] So far, the analysis and detection method of L-diethyl glutamate has not been recorded in the literature, but the analysis and detection of L-diethyl glutamate plays an important role in reaction control and yield improvement, and also directly affects The quality of the final product, so it is necessary to establish a stable and effective analytical method for quality control of L-diethyl glutamate

Method used

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  • Analysis and detection method of L-diethyl glutamate
  • Analysis and detection method of L-diethyl glutamate
  • Analysis and detection method of L-diethyl glutamate

Examples

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Embodiment 1

[0029] Instruments and conditions: Agilent1200 liquid chromatography system, VWD detector, chromatographic column: Yuexu XB-C18 (4.6×150mm, 5μm), detection wavelength 210nm, column temperature 27°C, flow rate 1.0mL / min, 0.05mol / L Sodium dihydrogen phosphate solution: 0.05 mol / L disodium hydrogen phosphate solution: acetonitrile in a volume ratio of 80:5:15 to form a mobile phase (pH 7.0).

[0030] Experimental procedure: Dissolve L-diethyl glutamate with mobile phase and quantitatively dilute to make a solution containing 20 mg of L-diethyl glutamate per 1 mL, as the test solution, and accurately measure the test solution 20 μL was injected into the liquid chromatograph, and the high-performance liquid chromatography was analyzed according to the above conditions, and the chromatogram was recorded. The results are shown in the attached figure 1 .

[0031] attached figure 1 It shows that under the chromatographic conditions, the peak of L-diethyl glutamate and impurity peaks ...

Embodiment 2

[0033] Instruments and conditions: Agilent1200 liquid chromatography system, VWD detector, chromatographic column: Yuexu XB-C18 (4.6×150mm, 5μm), detection wavelength 210nm, column temperature 27°C, flow rate 0.7mL / min, 0.05mol / L Sodium dihydrogen phosphate solution: 0.05mol / L disodium hydrogen phosphate solution: acetonitrile in a volume ratio of 70.5:4.5:25 to form a mobile phase (pH 7.0).

[0034] Experimental procedure: Dissolve L-diethyl glutamate with mobile phase and quantitatively dilute to make a solution containing 20 mg of L-diethyl glutamate per 1 mL, as the test solution, and accurately measure the test solution 20 μL was injected into the liquid chromatograph, and the high-performance liquid chromatography was analyzed according to the above conditions, and the chromatogram was recorded. The results are shown in the attached figure 2 .

[0035] attached figure 2 It shows that under the chromatographic conditions, the peak of L-diethyl glutamate and the peak o...

Embodiment 3

[0037] Instruments and conditions: Agilent1200 liquid chromatography system, VWD detector, chromatographic column: Yuexu XB-C18 (4.6×150mm, 5μm), detection wavelength 210nm, column temperature 27°C, flow rate 1.2mL / min, 0.05mol / L Sodium dihydrogen phosphate solution: 0.05mol / L disodium hydrogen phosphate solution: acetonitrile in volume ratio 84.6:5.4:10 to form mobile phase (pH value 7.0).

[0038] Experimental procedure: Dissolve L-diethyl glutamate with mobile phase and quantitatively dilute to make a solution containing 20 mg of L-diethyl glutamate per 1 mL, as the test solution, and accurately measure the test solution 20 μL was injected into the liquid chromatograph, and the high-performance liquid chromatography was analyzed according to the above conditions, and the chromatogram was recorded. The results are shown in the attached image 3 .

[0039] attached image 3 It shows that under this chromatographic condition, the peak of L-diethyl glutamate and the peak of i...

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Abstract

The invention relates to an analysis and detection method of L-diethyl glutamate and is used in quality control of the L-diethyl glutamate. Analysis and detection are carried out through HPLC, of which chromatographic conditions are described as follows: a chromatographic column (C18, 4.6*150mm, 5[mu]m) is filled with octadecylsilane chemically bonded silica as a filling material; a mobile phase is a solution system prepared by mixing a buffer salt solution and acetonitrile and regulating a pH value to 7.0 with NaOH; a detection wavelength is 210 nm; and a column temperature is 22-32 DEG C. By means of the analysis and detection method, the L-diethyl glutamate can be effectively separated out from impurities thereof. The method is high in separation degree, is simple in operations, is good in repeatability and durability, and is stable and reliable in results.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography analysis method, in particular to an analysis and detection method of L-diethyl glutamate. Background technique [0002] Pemetrexed disodium, developed by Eli Lilly Company of the United States, is a new type of multi-target folic acid blocker, which can block various enzymes required in the process of cancer cell division and proliferation, and even inhibit cell thymidine and purine nuclei. The activity of all folate-dependent enzymes is included in the biosynthesis of glycosides, and it is used in the treatment of malignant pleural mesothelioma and non-small cell lung cancer. [0003] L-diethyl glutamate is an important intermediate for the synthesis of pemetrexed disodium, and its chemical formula is C 9 h 17 NO 4 , the structural formula is as follows: [0004] [0005] So far, the analysis and detection method of L-diethyl glutamate has not been recorded in the literature, bu...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 赵志全
Owner SHANDONG NEWTIME PHARMA
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