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Method for detecting dehydrogenized vitamin C in vitamin C

A vitamin and dehydrogenation technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low sensitivity, low sensitivity, loss of vitamin C, etc., and achieve the effect of good repeatability and high sensitivity

Active Publication Date: 2016-09-28
JINAN KANGHE MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Since vitamin C is easily oxidized and decomposed to lose the efficacy of vitamin C, the minimum detection limit of dehydrovitamin C in the above detection methods is relatively high, the sensitivity is not high, and the recovery rate of the method exceeds 101%. In addition, amino column and silica gel The durability of the column is not high, the popularity of the evaporative light detector is poor, and the sensitivity is low. There is an urgent need for an analytical method with high sensitivity, low detection limit, and accurate recovery to detect dehydrovitamin C in vitamin C.

Method used

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  • Method for detecting dehydrogenized vitamin C in vitamin C
  • Method for detecting dehydrogenized vitamin C in vitamin C
  • Method for detecting dehydrogenized vitamin C in vitamin C

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The detection of embodiment 1 limit of detection and limit of quantitation

[0037] Step (1), accurately weigh 19.91 mg of the dehydrogenated VC reference substance (95.0%), put it in a 25ml measuring bottle, add mobile phase B to dissolve and dilute to the mark, and shake well;

[0038] Step (2), accurately measure 1ml of the solution in step (1), put it in a 100ml measuring bottle, add mobile phase B to dilute to the mark, and shake well;

[0039] Step (3), accurately measure 5ml of the solution in step (2), put it in a 100ml measuring bottle, add mobile phase B to dilute to the mark, shake well, and use it as the solution to be tested;

[0040] In step (4), 20 μl is accurately measured and injected into a liquid chromatograph, the signal-to-noise ratio S / N=10:1, and the solution is used as the quantification limit solution, and the quantification limit concentration is 0.38 μg / ml;

[0041] Step (5), accurately measure 3ml of the limit of quantitation solution, put i...

Embodiment 2

[0042] The determination of embodiment 2 standard curve

[0043] Step (1), accurately weigh 40.90 mg of the dehydrogenated VC reference substance (95.0%), put it in a 50ml measuring bottle, add mobile phase B to dissolve and dilute to the mark, shake well, and use it as the reference substance stock solution;

[0044] Step (2), accurately measure 2.5ml, 4ml, 5ml, 6ml, 7.5ml, and 10ml of the solution in step (1), put them in 100ml measuring bottles, add mobile phase B to dilute to the mark, shake well, and use them as linear Solution 1, linear solution 2, linear solution 3, linear solution 4, linear solution 5, linear solution 6;

[0045] Step (3) Accurately measure 20 μl each of the linear solutions 1-6 in step (2), inject into the liquid chromatograph, including the limit of quantification, take the concentration as the abscissa, and the peak area as the ordinate, perform linear regression, linear The equation is A=4.3953C-2.9546, the unit of C is ug / ml, A is the peak area; ...

Embodiment 3

[0046] Embodiment 3 Dehydrogenated VC recovery rate is measured

[0047] Step (1), weigh about 0.4g of VC raw material, put it in a 10ml measuring bottle, add mobile phase B to dissolve and dilute to the mark, shake well, and use it as the solution to be tested; accurately weigh the dehydrogenated VC reference substance (with a content of 95.0 %) 11.63mg, put in a 25ml measuring bottle, add mobile phase B to dissolve and dilute to the mark, shake well, as the reference substance stock solution, accurately measure 1ml, put in a 10ml measuring bottle, add mobile phase B to dilute to the mark, shake Uniform, as the reference substance solution;

[0048] Step (2): Accurately weigh three parts of about 0.4g of VC raw material, put each in a 10ml measuring bottle, add 0.8ml, 1.0ml, and 1.2ml of the reference substance stock solution respectively, dissolve and dilute to the mark with mobile phase B, shake Evenly, as 80%, 100%, and 120% group test solution respectively, each concentr...

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Abstract

The invention discloses a method for detecting dehydrogenized vitamin C in vitamin C and belongs to the field of analytic chemistry. The method is characterized in that the method uses liquid chromatography and an HILIC affinity chromatography column and uses acetonitrile--isopropanol-water as the mobile phase A and acetonitrile-water as the mobile phase B to perform analysis through gradient elution. The method has the advantages that by the method, the content of the dehydrogenized vitamin C can be analyzed fast and accurately; the quantification limit of the method can reach 0.38 microgram / ml, the detection limit of the method is 0.11 microgram / ml, the average yield of the method is 100.5%, and the concentration of the dehydrogenized vitamin C and peak area present a good linear relation in the range from 0.38 microgram / ml to 77.75 microgram / ml; the liquid-phase method is also applicable to vitamin quality researches such as researches on the stability and degradation of vitamin C medicine, compound vitamin (3) for injection and compound vitamin (13) injection.

Description

technical field [0001] The invention relates to a method for detecting dehydrovitamin C in vitamin C, in particular to a method for determining dehydrovitamin C by using a HILIC affinity column. Background technique [0002] Vitamin C is a catalyst in the oxidation-reduction reaction of cells. The human body cannot synthesize it by itself and must be ingested from food; adding vitamin C to food has multiple functions such as nutritional enhancement, anti-deterioration, and freshness preservation; its structural formula is: [0003] [0004] Molecular formula is C 6 h 8 o 6 , the molecular weight is 176.13 [0005] Vitamin C is unstable and easily decomposed by oxidation, thus losing the efficacy of vitamin C. When under aerobic conditions, vitamin C is oxidized to dehydroascorbic acid (dehydroascorbic acid), which then produces 2,3-dioxo-L-gulonic acid (2,3-Dike-to-L-gulonic acid), and further degrade to generate furfural and hydroxyfurfural; the generation of dehydr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/02G01N30/06G01N30/74
CPCG01N30/02G01N30/06G01N30/74G01N30/88G01N2030/027G01N2030/062G01N2030/884
Inventor 张颖李永福姜明明翟雪梅朱召贞
Owner JINAN KANGHE MEDICAL TECH
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