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Method for analyzing and detecting pemetrexed disodium intermediate

A technology for pemetrexed disodium and pemetrexed disodium, which is applied in the field of high performance liquid chromatography analysis, can solve problems such as affecting the quality of final products, and achieve stable and reliable results, good linear relationship, repeatability and durability good effect

Active Publication Date: 2014-06-25
SHANDONG NEWTIME PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] So far, USP, EP, BP, JP and Chinese Pharmacopoeia and literature do not record the analysis and detection method of pemetrexed disodium intermediate, but the analysis and detection of pemetrexed disodium intermediate has a great impact on reaction control and yield. The improvement of the yield plays an important role, 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 the pemetrexed disodium intermediate

Method used

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  • Method for analyzing and detecting pemetrexed disodium intermediate
  • Method for analyzing and detecting pemetrexed disodium intermediate
  • Method for analyzing and detecting pemetrexed disodium intermediate

Examples

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Embodiment 1

[0031] Instruments and conditions: Agilent1200 liquid chromatography system, VWD detector, chromatographic column: Agilent Extend-C18 (4.6×250mm, 5μm); detection wavelength: 254nm; column temperature: 25°C; flow rate: 1.0mL / min; 0.0265mol / L Potassium dihydrogen phosphate solution and acetonitrile in a volume ratio of 68:32 were used as the mobile phase.

[0032] Experimental procedure: dissolve the pemetrexed disodium intermediate with mobile phase and quantitatively dilute to make a solution containing 0.5 mg of pemetrexed disodium intermediate in every 1 mL, as the test solution; accurately measure the test product 20 μL of the solution 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 .

[0033] attached figure 1 It shows that under the chromatographic conditions, the pemetrexed disodium intermediate pea...

Embodiment 2

[0035] Instruments and conditions: Agilent1200 liquid chromatography system, VWD detector, chromatographic column: Agilent Extend-C18 (4.6×250mm, 5μm); detection wavelength: 254nm; column temperature: 25°C; flow rate: 0.7mL / min; 0.01mol / L Potassium dihydrogen phosphate solution and acetonitrile in a volume ratio of 58:42 were used as the mobile phase.

[0036] Experimental procedure: dissolve the pemetrexed disodium intermediate with mobile phase and quantitatively dilute to make a solution containing 0.5 mg of pemetrexed disodium intermediate in every 1 mL, as the test solution; accurately measure the test product 20 μL of the solution 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 .

[0037] attached figure 2 It shows that under the chromatographic conditions, the pemetrexed disodium intermediate pea...

Embodiment 3

[0039] Instruments and conditions: Agilent1200 liquid chromatography system, VWD detector, chromatographic column: Agilent Extend-C18 (4.6×250mm, 5μm); detection wavelength: 254nm; column temperature: 25°C; flow rate: 1.2mL / min; 0.04mol / L Potassium dihydrogen phosphate solution and acetonitrile in a volume ratio of 75:25 were used as the mobile phase.

[0040] Experimental procedure: dissolve the pemetrexed disodium intermediate with mobile phase and quantitatively dilute to make a solution containing 0.5 mg of pemetrexed disodium intermediate in every 1 mL, as the test solution; accurately measure the test product 20 μL of the solution 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 .

[0041] attached image 3 It shows that under the chromatographic conditions, the pemetrexed disodium intermediate peak ...

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Abstract

The invention relates to a method for analyzing and detecting a pemetrexed disodium intermediate. The method is used for quality control of the pemetrexed disodium intermediate. According to the method, octadecylsilane chemically bonded silica serves as a chromatographic column of packing (C18, 4.6*250mm, 5 micrometers), a monopotassium phosphate solution and acetonitrile serve as a mobile phase, the detection wavelength is 249-259nm, and high performance liquid chromatography is performed for analysis and detection. According to the analysis and detection method, the pemetrexed disodium intermediate can be effectively separated from impurities thereof, and the method has the advantages of high separation degree, good linear relation, simple operation, high repeatability and durability and stable and reliable result.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography analysis method, in particular to an analysis and detection method of a pemetrexed disodium intermediate. 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] N-[4-[2-(2-amino-4,7-dihydro-4-oxo-1H-pyrrolo[2,3-d]pyrimidin-5-yl)ethyl]benzoyl]- L-diethyl glutamate p-toluenesulfonate is an important intermediate for the synthesis of pemetrexed disodium, its chemical formula is C31H37N5O9S, and its structural formula is as follows: [0004] [00...

Claims

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Application Information

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