A method for rapid screening of folic acid by high performance thin layer chromatography-gas fluorescence derivatization

A thin-layer chromatography, fluorescence technology, applied in fluorescence/phosphorescence, material analysis by optical means, material excitation analysis, etc., can solve problems such as unfavorable applications

Active Publication Date: 2019-07-02
JIANGNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The solution oxidation method is not conducive to the application in flat thin layer chromatography. Therefore, it is urgent to establish an oxidation pretreatment method suitable for high performance thin layer chromatography to achieve efficient and rapid detection of folic acid on thin layer chromatography.

Method used

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  • A method for rapid screening of folic acid by high performance thin layer chromatography-gas fluorescence derivatization
  • A method for rapid screening of folic acid by high performance thin layer chromatography-gas fluorescence derivatization
  • A method for rapid screening of folic acid by high performance thin layer chromatography-gas fluorescence derivatization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Preparation of folic acid standard solution: use 1% ammonia water as a solvent, dilute with methanol to prepare a folic acid standard solution with a concentration of 0.01 mg / mL;

[0024] (2) High-efficiency thin-layer chromatography separation: 2-8 μL folic acid standard and multivitamin tablet / breakfast cereal / feed sample are accurately sampled with Linomat 5, and after sample pointing is completed, use a developing solution (methanol / ethyl acetate / three Ethylamine / water=6 / 4 / 1 / 1(v / v)) to expand, expand upward for 60mm, take out the silica gel plate and place it on a flat heater at 50°C for 3 minutes to fully dry;

[0025] (3) Folic acid oxidation fluorescence: put the silica gel plate under normal temperature and pressure, containing 20-22cm 3 / m 3 Bromine gas and the rest are oxidized in a closed environment of air for a certain period of time to generate fluorescent products, take out the silica gel plate, and place it under the irradiation of a 366nm ultraviol...

Embodiment 2

[0028] The specific embodiment is the same as Example 1, the difference is that the oxidation time is respectively 0min, 3min, 5min, 10min, 15min, and the results are as follows figure 2 shown. The fluorescent bands were stronger when oxidized for 3min and 5min, and weaker at 10min and 15min.

Embodiment 3

[0030] (1) Test the folic acid in vitamin pills, breakfast cereals and feed respectively.

[0031] Pretreatment of multivitamin tablets: Grind the tablets, weigh 0.5g and dissolve them in 10ml of 1% ammonia water, take them out after ultrasonication for 20min, centrifuge at 3500r / min for 10min, pass through a 0.45μm water film to obtain tablet samples, and refrigerate at 4°C.

[0032] Pretreatment of breakfast cereals: grind the cereals separately, weigh 2.5g, add 10ml of 0.1mol / L hydrochloric acid, put them in an autoclave and heat at 121°C for 15min. Take it out and cool it to room temperature, adjust the pH to 6.8-7.2 with 1mol / L sodium hydroxide, add 1mL of peak amylase and place it at 37°C for 4h. After the end, dilute to 50 mL with methanol. After centrifugation, the supernatant was passed through a membrane to obtain a grain sample, which was refrigerated at 4°C.

[0033] Feed pretreatment is the same as breakfast cereals.

[0034] (2) Using 0.5MPa nitrogen gas as th...

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Abstract

The invention discloses a method for rapidly screening folic acid by high-performance thin layer chromatography-gas phase fluorescence derivatization, and belongs to the technical field of food detection. According to the characteristic of folic acid without fluorescence, an in-situ gas oxidation fluorescence derivatization method is established to carry out a derivatization reaction on a sample to be tested, HPTLC is used as an open chromatographic separation carrier, and then scanning quantification is carried out by using a thin layer chromatography scanner. The method provided by the invention has the advantages of short detection period and good accuracy; a single screening process needs only 1-2h from sample preparation to obtain a final result; the detection limit can reach 20-50mug / kg; the detection method can realize that the repeatability RSD is less than 10%; and the detection result is basically consistent with an HPLC detection result.

Description

technical field [0001] The invention relates to a high-efficiency thin-layer chromatography-gas phase fluorescence derivation rapid screening method for folic acid, which belongs to the technical field of food detection. Background technique [0002] Folic acid (also known as vitamin B9), the molecular structure is composed of pteridine p-aminobenzoic acid and L-glutamic acid, is a B vitamin with important physiological functions, and has important nutrition for human health and livestock and poultry breeding value. At present, there are many kinds of folic acid supplements and functional foods on the market, the quality is uneven, and there are many problems such as false labeling of folic acid content. Therefore, research on a rapid quantitative method of folic acid has become an urgent problem to be solved in the monitoring of folic acid supplements and related food and drug in food and drug. [0003] At present, the common detection method of folic acid in food and med...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/90G01N21/64
CPCG01N21/6428G01N30/90
Inventor 陈益胜徐学明王萍谢正军杨哪吴凤凤金亚美
Owner JIANGNAN UNIV
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