Method for determining vitamins A, D and E in milk powder

A vitamin and milk powder technology, applied in the field of analytical chemistry, can solve problems such as the inability to meet the test requirements of low-content samples, difficulty in lowering the detection limit of VD, matrix interference, etc., to achieve automatic online purification detection, ensure accuracy and reproducibility, Ensures accuracy and reproducibility of results

Active Publication Date: 2018-10-16
SGS STANDARD TECHNICAL SERVICES SHANGHAI CO LTD
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0005] In 2013, Wang Anqun et al. reported a method for the determination of vitamin A, D3, and E in feed by high-performance liquid chromatography in the journal "Environmental Monitoring Management and Technology". The matrix is ​​complex, which seriously damages the chromatographic column. At the same time, the low VD content is easily interfered by the matrix and cannot be detected, so it is difficult to popularize
However, its pre-treatment must be avoided through saponification, wall-breaking extraction, organic solvent phase inversion, and concentration of these tedious processes
Although the two-dimensional column switching method solves the problem of matrix interfe

Method used

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  • Method for determining vitamins A, D and E in milk powder
  • Method for determining vitamins A, D and E in milk powder
  • Method for determining vitamins A, D and E in milk powder

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Embodiment 1

[0042] Embodiment 1: the mensuration of vitamin A in milk powder, D, E

[0043] 1. Sample preparation:

[0044] Accurately weigh 2g of the mixed sample into a 150mL flat-bottomed flask, add 20mL of distilled water, 30mL of absolute ethanol, 1g of ascorbic acid, 1g of BHT, 20mL of 50% KOH aqueous solution, heat in a water bath at 80°C for 30min, cool to room temperature after completion, and use 50% Dilute ethanol water solution to 100mL, take 2mL through a 0.45μm filter membrane, and analyze on the machine.

[0045] 2. Set the instrument parameters:

[0046] The operating conditions of the online solid phase extraction part are:

[0047] (1) The vitamin A, D, E enrichment purification column adopts PLRP-S column, the specification is 4.6×12.5mm, and the pore size is 15-20um;

[0048] (2) The mobile phase is 40% ethanol aqueous solution, and the running time is 22min; the mobile phase flow rate: 0-4min is 1mL / min; 4-15min is 0.2mL / min; 15-22min is 1mL / min, and the injection ...

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Abstract

The invention relates to a method for determining vitamins A, D and E in milk powder. The method comprises the steps as follows: uniformly mixing a milk powder sample, weighing a proper quantity of the milk powder sample, adding water, absolute ethyl alcohol, ascorbic acid, BHT and KOH aqueous solutions, performing heating saponification, and performing cooling and diluting to a specified volume after saponification; determining the content of vitamins A, D and E in the solution by an HPLC (high performance liquid chromatograph) with a double-valve and three-pump system; determining whether vitamins A and E exist in the sample or not by comparing the retention time of the sample and a standard substance in one-dimensional liquid chromatography; determining whether vitamin D exists in the sample or not by comparing the retention time of the sample and the standard substance in two-dimensional liquid chromatography; calculating the content of vitamins A, D and E in the sample according to the amounts of vitamins A, D and E after conversion. The operation steps are simplified, the pretreatment time is greatly shortened, the labor and reagent costs are saved, automatic online purification detection is realized, the sensitivity is improved, and the accuracy and reproducibility of test results are guaranteed.

Description

[technical field] [0001] The invention belongs to the technical field of analytical chemistry, in particular to a method for determining vitamins A, D and E in milk powder. [Background technique] [0002] Vitamins widely exist in various organisms, and about dozens of types have been discovered so far, with different chemical structures, including aliphatic, aromatic, alicyclic, heterocyclic and steroidal compounds. In terms of physiological functions, they are neither the main raw materials for various tissues nor the source of energy in the body, but they are small molecular organic compounds that are essential to participate in the mediation of substance metabolism. Vitamins A, D, and E are all non-polar hydrophobic isoprene derivatives, soluble in lipids and fat solvents, but insoluble in water, and belong to fat-soluble vitamins. Excessive intake, unbalanced intake or lack of intake will cause corresponding symptoms, affecting the growth and development of the body and...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/74G01N30/88G01N30/60
CPCG01N30/02G01N30/06G01N30/60G01N30/74G01N30/88G01N2030/027G01N2030/062G01N2030/884
Inventor 李丹杨新磊周洁李浪关玲玲陈建彪
Owner SGS STANDARD TECHNICAL SERVICES SHANGHAI CO LTD
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