Detection method for liquid chromatogram of keto-L-gulonic acid and/or keto-L-gulonic acid methyl ester

A technology of methyl gulonate and a detection method, applied in the field of high performance liquid chromatography detection of gulonic acid and/or methyl gulonate, can solve problems such as inability to accurately quantify, and achieve lower detection limit, true and reliable detection results, and ease of use. effect of operation

A technology of methyl gulonate and a detection method, applied in the field of high performance liquid chromatography detection of gulonic acid and/or methyl gulonate, can solve problems such as inability to accurately quantify, and achieve lower detection limit, true and reliable detection results, and ease of use. effect of operation

CN102495165AActive Publication Date: 2012-06-13安徽泰格生物技术股份有限公司
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  • Detection method for liquid chromatogram of keto-L-gulonic acid and/or keto-L-gulonic acid methyl ester
  • Detection method for liquid chromatogram of keto-L-gulonic acid and/or keto-L-gulonic acid methyl ester
  • Detection method for liquid chromatogram of keto-L-gulonic acid and/or keto-L-gulonic acid methyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 Detection of Gulonic Acid Content

[0031] 1. Reagents and solutions

[0032] 1. Gulonic acid standard product: purity ≥ 99.0%.

[0033] 2.0.025mol / L Potassium Dihydrogen Phosphate Solution: Take 3.4g of Potassium Dihydrogen Phosphate, add appropriate amount of water to dissolve into 1000mL, and shake well.

[0034] 3. Guronic acid standard solution: take 0.10 g of gulong acid standard product, weigh it accurately, put it in a 100 mL volumetric flask, dissolve it with 0.025 mol / L potassium dihydrogen phosphate solution and dilute to the mark, the concentration of this solution is 1 mg / mL.

[0035] 2. Instruments and equipment

[0036] 1. Analytical balance: the sensitivity is 0.0001g.

[0037] 2. Microporous membrane: pore size 0.45μm.

[0038] 3. High performance liquid chromatography (equipped with ultraviolet detector).

[0039] 3. Analysis steps

[0040] 1. High performance liquid chromatography conditions

[0041] Chromatographic column: Sinochrom ...

Embodiment 2

[0064] 1. Reagents and solutions

[0065] 1. Gulonic acid standard product: purity ≥ 99.0%.

[0066] 2. Standard product of methyl guronate: purity ≥ 99.0%.

[0067] 3.0.025mol / L Potassium Dihydrogen Phosphate Solution: Take 3.4g of Potassium Dihydrogen Phosphate, add appropriate amount of water to dissolve into 1000mL, and shake well.

[0068] 4. Mixed standard solution: take about 0.10 g of the standard product of gulong acid and about 1.0 g of the standard product of methyl guronate, respectively, weigh them accurately, put them in a 100 mL volumetric flask, dissolve them with 0.025 mol / L potassium dihydrogen phosphate solution and make to volume to scale. The concentration of guronic acid in this solution is 1 mg / mL, and the concentration of methyl guronate is 10 mg / mL.

[0069] 2. Instruments and equipment

[0070] 1. Analytical balance: the sensitivity is 0.0001g.

[0071] 2. Microporous membrane: pore size 0.45μm.

[0072] 3. High performance liquid chromatography...

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Abstract

The invention relates to a detection method for liquid chromatogram of keto-L-gulonic acid and / or keto-L-gulonic acid methyl ester. Detection results of a standard sample and a sample to be detected can be respectively obtained by means of detection through a liquid chromatogram mode under the same condition, and contents of the keto-L-gulonic acid and / or the keto-L-gulonic acid methyl ester in the sample to be detected is calculated out through an external standard method. Under the condition of the same chromatogram, the detection method can not only respectively detect the keto-L-gulonic acid and the keto-L-gulonic acid methyl ester independently, but also detect mixture of the keto-L-gulonic acid and the keto-L-gulonic acid methyl ester, thereby establishing a quick and accurate quantitative detection method. The detection method is especially suitable for detecting quantity of surplus keto-L-gulonic acid and the keto-L-gulonic acid methyl ester in methyl esterification reaction coarse products of the keto-L-gulonic acid, and can quantitatively and accurately inspect the reaction process and yield of target products. The detection method is simple and easy to operate, and detection results are authentic and reliable.

Description

technical field [0001] The invention relates to the field of analytical chemistry detection, in particular to a high-performance liquid chromatography detection method for gulonic acid and / or guronate methyl ester. Background technique [0002] Vitamin C is a water-soluble vitamin essential to the human body. The main raw material for the production of vitamin C, sorbitol, is fermented, extracted, and concentrated to obtain solid gulonic acid, which is transformed by alkali to obtain crude vitamin C, and then refined to obtain finished vitamin C. 2-Keto-L-methyl guronate (hereinafter referred to as "methyl guronate") is a precursor for the synthesis of vitamin C, and methyl guronate is the product of methyl esterification reaction in the first step of vitamin C base conversion process , this step reaction is an esterification reaction under the action of acid catalysis, which is a reversible reaction. In order to investigate the yield and quality of intermediates, the hydr...

Claims

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Application Information

Patent Timeline
13 Jun 2012
Publication
CN102495165A
IPC
G01N30/88
Inventors
芦光洪; 常珠侠