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High-performance liquid phase method capable of simultaneously detecting gulconic acid, gulconic methyl ester, methanol and ethanol

A technology of methyl guronate and high performance liquid phase, which is applied in the field of chemical analysis, can solve qualitative and quantitative problems, and achieve the effects of good reproducibility, fast detection speed and high sensitivity

Active Publication Date: 2013-10-09
NORTHEAST PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] It can be seen that the current research cannot simultaneously carry out qualitative and quantitative analysis of gulonic acid, methyl guronate, methanol and ethanol in the production of vitamin C. The high-performance liquid phase method has been an urgent problem to be solved

Method used

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  • High-performance liquid phase method capable of simultaneously detecting gulconic acid, gulconic methyl ester, methanol and ethanol
  • High-performance liquid phase method capable of simultaneously detecting gulconic acid, gulconic methyl ester, methanol and ethanol
  • High-performance liquid phase method capable of simultaneously detecting gulconic acid, gulconic methyl ester, methanol and ethanol

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Experimental program
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preparation example Construction

[0032] (2) Preparation of standard solution

[0033] Accurately weigh an appropriate amount of standard product, dilute to a certain concentration with mobile phase, and filter to obtain a standard product solution;

[0034] (3) Preparation of the test solution

[0035] Accurately weigh an appropriate amount of the test product, dilute it to a certain concentration with the mobile phase, and filter to obtain the test product solution;

[0036] (4) Determination

[0037] Standard solution and need testing solution are carried out high-performance liquid chromatography detection respectively, wherein the separation degree between the peaks to be detected in need testing solution is greater than 1.5, obtain standard solution chromatogram and need testing solution chromatogram respectively, according to standard The peak time of the product and the test product is used to characterize the components of the test product, and the content of the components to be detected is obtaine...

Embodiment 1

[0052] Method for detection of components and content of esterification liquid

[0053] Equipment: Waters liquid chromatograph, including 1525 binary gradient pump, 2414 refractive index detector, 2707 autosampler, chromatographic column HPX-87H (specification 300×7.8mm). Workstation: Empower.

[0054] Mobile phase: 0.05mol / L dilute sulfuric acid aqueous solution; flow rate: 0.4ml / min; column temperature: 40°C; injection volume: 20μl. Sample response time is 40min.

[0055] Preparation of the solid standard solution: Accurately weigh 10 mg of the standard product of guronic acid and 10 mg of the standard product of methyl guronate, respectively, and quantitatively prepare a solution of guaronic acid with a concentration of 0.05 mg / ml and a standard product of 0.05 mg / ml with a mobile phase. Methyl guronate solution was filtered through a 0.22 μm microporous membrane to obtain a standard solution of guronate with a concentration of 0.05 mg / ml and a standard solution of methyl...

Embodiment 2

[0073] The detection method of the composition and content of the methanol washing solution of guronic acid

[0074] Equipment: Waters liquid chromatograph, including 1525 binary gradient pump, 2414 refractive index detector, 2707 autosampler, chromatographic column HPX-87H (specification 300×7.8mm). Workstation: Empower.

[0075] Mobile phase: 0.05mol / L dilute sulfuric acid aqueous solution; flow rate: 0.4ml / min; column temperature: 40°C; injection volume: 20μl. Sample response time is 40min.

[0076] Preparation of the solid standard solution: Accurately weigh 10 mg of the standard product of guronic acid and 10 mg of the standard product of methyl guronate, respectively, and quantitatively prepare a solution of guaronic acid with a concentration of 0.05 mg / ml and a standard product of 0.05 mg / ml with a mobile phase. Methyl guronate solution was filtered through a 0.22 μm microporous membrane to obtain a standard solution of guronate with a concentration of 0.05 mg / ml and ...

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Abstract

The invention provides a high-performance liquid phase method capable of simultaneously detecting gulconic acid, gulconic methyl ester, methanol and ethanol. The method comprises the following steps of: chromatographic conditions: taking a polystyrene-divinylbenzene resin column as a chromatographic column and a dilute acid aqueous solution as a moving phase, and taking a differential refraction detector as a detector; preparation of a standard sample solution preparation: accurately weighing appropriate standard sample, diluting the standard sample by using the moving phase until the standard sample has a certain concentration, and filtering so as to obtain the standard sample solution; preparation of a test sample solution preparation: accurately weighing appropriate test sample, diluting the test sample by using the moving phase until the standard sample has a certain concentration, and filtering so as to obtain the test sample solution; measurement: respectively performing high-performance liquid chromatography on the standard sample solution and the test sample solution, determining the chemical compositions of the test sample according to the appearance time of the standard sample and the appearance time of the test sample, and calculating according to an external standard method, thereby obtaining the content of a component to be tested. The high-performance liquid phase method is capable of performing qualitative and quantitative analysis on a plurality of components such as gulconic acid, gulconic methyl ester, methanol and ethanol simultaneously and has the advantages of high detection speed, high detection data accuracy, good repeatability, high sensitivity, and simple and convenient operation.

Description

technical field [0001] The invention relates to the simultaneous detection of multiple components in the field of chemical analysis, in particular to a high-efficiency liquid phase method capable of simultaneously detecting guronic acid, methyl guronate, methanol and ethanol. Background technique [0002] Vitamin C is an important raw material in the pharmaceutical and food industries. At present, vitamin C is mainly produced by the Reyes method or two-step fermentation in industry. In the process of producing vitamin C by two-step fermentation method, the qualitative and quantitative analysis of guronic acid, methyl guronate, methanol and ethanol is carried out on the intermediate guronic acid ultrafiltrate or guronic acid methyl ester solid etc. for the process of vitamin C production Control and finished product quality of vitamin C are critical. Gulonic acid is also called 2-keto-L-gulonic acid, and methyl guronate is also called 2-keto-L-gulonic acid methyl ester. [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 刘宇浩徐莉张海宏谢占武胡昊赵利军王国君敖志刚
Owner NORTHEAST PHARMA GRP