Column for separating and purifying micromolecular pollutant in food and application method thereof

A technology for small molecules and pollutants, which is applied in the direction of chemical instruments and methods, other chemical processes, and the preparation of test samples. It can solve the problems of labor cost and time-consuming, and achieve simple and labor-saving operation, good purification effect, and convenient use. quick effect

Inactive Publication Date: 2015-04-22
ZHEJIANG CENT FOR DISEASE CONTROL & PREVENTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These substances may exist in whole or in part in the same food (such as dairy products, high-temperature processed foods, condiments, and cooked dietary samples, etc.). Existing methods require multiple methods because of their different polarities and functional groups. The two methods are extracted separately and detected separately, which is time-consuming, laborious and costly

Method used

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  • Column for separating and purifying micromolecular pollutant in food and application method thereof
  • Column for separating and purifying micromolecular pollutant in food and application method thereof
  • Column for separating and purifying micromolecular pollutant in food and application method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Object to be inspected: soy sauce;

[0039] Types of small-molecule food contaminants: urethane, 4 kinds of chloropropanol, acrylamide;

[0040] Purification column packing configuration: packing 2g, of which the upper layer of diatomaceous earth (Extrelut TM NT, Merck Chemical Technology (Shanghai) Company) 1.5g, Amine-based fillers (NH2, Aigel Technology (Tianjin)) 0.2g, lower layer of diatomaceous earth (Extrelut TM NT, Merck Chemical Technology (Shanghai) Company) 0.3g;

[0041] The purification method includes the following steps:

[0042] The first step is to load the sample. Accurately weigh 1g of the well-mixed soy sauce sample and directly add it to the purification column and let it stand for 20 minutes to make the sample liquid fully dispersed and adsorbed in the solid diatomaceous earth filler;

[0043] The second step is to rinse and remove impurities; add 10mL of n-hexane to rinse and discard;

[0044] The third step, elution, eluted with 15ml ethyl acetate: ether=...

Embodiment 2

[0048] Objects to be inspected: mixed meal samples;

[0049] Types of small-molecule food contaminants: urethane, 4 kinds of chloropropanol, acrylamide;

[0050] Purification column packing configuration: packing 5.5g, of which the upper layer of diatomaceous earth (Celite545) 4.5g, the amine-based packing (PSA, Aijieer Technology (Tianjin)) 0.5g, the lower layer of diatomaceous earth (Celite545) 0.5g;

[0051] The purification method includes the following steps:

[0052] The first step is to stir and mix the sample evenly, accurately weigh 0.5g of a well-mixed meal sample, add water-extract 2 times, add 2 mL of water each time;

[0053] The second step is to load the sample. Combine the extracts obtained after the two extractions and add them directly to the purification column, and let it stand for 30 minutes to make the sample liquid fully dispersed and adsorbed in the solid-phase diatomaceous earth filler;

[0054] The second step is to rinse and remove impurities; add 35 mL of n-he...

Embodiment 3

[0059] Objects to be inspected: liquid milk products;

[0060] Types of small-molecule food contaminants: ethyl carbamate, 4 kinds of chloropropanol, acrylamide, 3 kinds of milk flavor (ethyl maltol, vanillin, ethyl vanillin);

[0061] Packing configuration of purification column: same as in Example 1.

[0062] The purification method includes the following steps:

[0063] The first step is to load the sample, accurately weigh 1g of the uniformly mixed liquid milk product sample, directly add it to the purification column, and let it stand for 20 minutes to make the sample liquid fully dispersed and adsorbed in the solid diatomaceous earth filler. The other subsequent steps are the same Example 1;

[0064] Analyte recovery rate: The target analytes are 9 small-molecule food contaminants, which are detected by GC-MS / MS. The chromatograms of typical samples are shown in image 3 , Where EC: not detected, 1,3-DCP: not detected, 2,3-DCP: not detected, AA: 6.9μg / kg, 3-MCPD: 5.1μg / kg, 2-MCPD...

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Abstract

The invention provides a column for separating and purifying micromolecular pollutant in food. The column for separating and purifying micromolecular pollutant in food mainly comprises a column body, a filler filled in the column body and sieve plates arranged at the upper end and the lower end of the filler, wherein the filler is filled in layers and sequentially comprises an upper diatomite layer and an amino solid-phase extraction filler from top to bottom and also can comprises a lower diatomite layer. The particle size of the filler is 5-1000 micrometers; and the filler comprises the diatomite upper layer and the amino solid-phase extraction filler, wherein mass fraction of the upper diatomite layer is 50-95%, and the mass fraction of the amino solid-phase extraction filler is 5-50%. The invention also discloses a method for separating and purifying micromolecular pollutant in food by utilizing the separating and purifying column. The column and method for separating and purifying micromolecular pollutant in food have the advantages that a liquid sample is directly loaded or is simply dispersed and then loaded, operation is easy, labour is saved and a purifying column is low in cost and easy to manufacture; and a purifying method is quick, a purifying effect is good, and the purifying method is applicable to extraction and purification on micromolecular food pollutant containing a polar group in a complex matrix.

Description

(1) Technical field [0001] The invention relates to a purification column for simultaneous extraction of small molecule pollutants in food and a method for purifying a target measured substance in a sample by using the purification column. (2) Background technology [0002] Chloropropanol in condiments, fermented foods and high-temperature fried foods (including 1,3-DCP and 2,3-DCP two dichloropropanols and 3-MCPD and 2-MCPD two monochloropropanediols), amino Small molecule compounds such as ethyl formate (EC) and acrylamide (AA) are hot pollutants in the current food safety field. Vanillin milk flavors (including vanillin (VA), ethyl vanillin (EV) and Ethyl maltol (EW), etc.) has become the focus of food safety issues related to foreign milk powder because of its illegal addition in infant formula milk powder. These compounds include polar groups such as alcohols, carbamates, amides, phenolic hydroxyl groups and aldehydes. Among them, dichloropropanol and ethyl vanillin are rel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/14G01N1/34
Inventor 徐小民任一平黄百芬
Owner ZHEJIANG CENT FOR DISEASE CONTROL & PREVENTION
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