Method for detecting oxalic acid content in vitamin C

A vitamin and medium oxalic acid technology, applied in the field of analytical chemistry, can solve the problems of incomplete application, uncommonly used chromatographic columns, and unsatisfactory specificity, etc., and achieve the effect of high sensitivity and easy availability of consumables

Inactive Publication Date: 2020-05-15
JINAN KANGHE MEDICAL TECH
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Problems solved by technology

[0007] The vitamin C oxalic acid test method recorded in domestic and foreign pharmacopoeias is the turbidimetric method. For preparations containing vitamin C raw materials such as multivitamins for injection (12), due to the color of the sample solution, the turbidimetric method is not suitable. In Li Zhiwei et al. In the published reference "HPLC determination of oxalic acid in compound vitamins for injection", high performance liquid chromatography, strong cation exchange column (H + type) for the determination of oxalic acid, but this type of chromatographic column is not commonly used, and the specificity is not very ideal. Other literatures on the determination of vitamin C related substances control other simple impurities and total impurities, and do not control oxalic acid separately; The determination method of oxalic acid content in food is not fully applicable to vitamin C or preparations containing vitamin C

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  • Method for detecting oxalic acid content in vitamin C
  • Method for detecting oxalic acid content in vitamin C
  • Method for detecting oxalic acid content in vitamin C

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The detection of embodiment 1 detection limit and quantitative limit

[0036] Step (1) Take about 20mg of oxalic acid reference substance, weigh it accurately, put it in a 25ml measuring bottle, add water to dissolve and dilute to the mark, and shake well;

[0037] Step (2) Accurately measure 5ml of the solution in step (1), put it in a 50ml measuring bottle, dilute with water to the mark, and shake well;

[0038] Step (3) Accurately measure 0.5ml of the solution in step (2), place it in a 100ml measuring bottle, add water to dilute to the mark, shake well, accurately measure 50μl, inject it into a liquid chromatograph, the signal-to-noise ratio S / N is about is 10:1, as the limit of quantification, the concentration of oxalic acid is 0.8004μg / ml;

[0039] Step (4) Accurately measure 5ml of the solution in step (3), put it in a 10ml measuring bottle, add water to dilute to the mark, shake well, accurately measure 50μl, inject it into a liquid chromatograph, the signal-t...

Embodiment 2

[0040] The determination of embodiment 2 standard curve

[0041] Step (1) Take about 20mg of oxalic acid reference substance, weigh it accurately, put it in a 25ml measuring bottle, add water to dissolve and dilute to the mark, and shake well;

[0042] Step (2) Accurately measure 5ml of the solution in step (1), put it in a 50ml measuring bottle, dilute with water to the mark, and shake well;

[0043] Step (3) Accurately measure the solutions 1, 2, 3, 4, 5, and 6ml in step (2) respectively, put them in different 100ml measuring bottles, add water to dilute to the mark, shake well, and use them as 20%, 40%, 60% %, 80%, 100% and 120% linear solutions.

[0044] Step (4) Precisely measure 50 μl of the linear solution in step (3), inject it into the liquid chromatograph, take the concentration C (μg / ml) as the abscissa, and take the peak area A as the ordinate, and perform linear regression, see the instructions Attached picture figure 1 , the linear equation is A=30540C-208, an...

Embodiment 3

[0045] The mensuration of embodiment 3 recovery rate

[0046] Step (1) Take about 20mg of oxalic acid reference substance, weigh it accurately, put it in a 25ml measuring bottle, dissolve it with water and dilute to the mark, shake well, take 5ml precisely, put it in a 50ml measuring bottle, dilute with water to the mark, shake well, As oxalic acid reference substance stock solution;

[0047] Step (2) Accurately measure 5ml of the reference substance stock solution, put it in a 100ml measuring bottle, dilute it with water to the mark, shake it up, and use it as the oxalic acid reference substance solution;

[0048] Step (3) Take about 390mg of multivitamin (12) for injection, weigh it accurately, put it in a 50ml measuring bottle, add water to dissolve and dilute to the mark, shake well, and you get it.

[0049] Step (4) Take about 390 mg of multivitamins (12) for injection, accurately weighed, and put in three parts in total, put them in different 50ml measuring bottles resp...

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Abstract

The invention relates to an analysis method for detecting oxalic acid content; a high performance liquid chromatograph is adopted, and chromatographic conditions are as follows: an octadecylsilane chemically bonded silica chromatographic column is adopted, a mobile phase is phosphate buffered solution (containing tetrabutylammonium hydroxide)-acetonitrile, and the mobile phase A and the mobile phase B are carried out according to a gradient program; the flow rate is 0.9-1.6 ml/min; the column temperature is 28-40 DEG C, the detection wavelength is 200-210 nm, and the sample size is 20-50 [mu]l. The detection method has the advantages of high sensitivity and good linear relationship, and is suitable for detecting the oxalic acid content in vitamin C or preparations containing vitamin C.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a high-efficiency liquid phase analysis method for detecting oxalic acid content in vitamin C. Background technique [0002] Vitamin C (Vitamin C, Ascorbic Acid), also known as L-ascorbic acid, is a water-soluble vitamin. The main effect of vitamin C depends on enhancing immunity, preventing cancer, heart disease, stroke, protecting teeth and gums and so on. Oxalic acid is one of the main degradation products of vitamin C, which can reduce the bioavailability of mineral elements. It is easy to form calcium oxalate with calcium ions in the human body and cause kidney stones. Therefore, oxalic acid is often considered as an antagonist of mineral element absorption and utilization. Its structural formula is as follows respectively: [0003] Vitamin C [0004] [0005] oxalic acid [0006] [0007] The vitamin C oxalic acid test method recorded in domestic an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/30G01N30/32G01N30/36G01N30/60
CPCG01N30/02G01N30/30G01N30/32G01N30/36G01N30/60G01N2030/324
Inventor 翟雪梅许庆栋蒋硕于珊珊刁婷陈俏王卫陶冶张颖
Owner JINAN KANGHE MEDICAL TECH
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