Dynamic superheated liquid water extraction device and method for veterinany drug residues in food

An extraction device, a technology for agricultural and veterinary drugs, applied in chemical instruments and methods, measuring devices, separation methods, etc., to ensure continuity, be beneficial to the protection of health and the environment, and overcome low extraction efficiency.

Inactive Publication Date: 2012-07-04
ANIMAL & PLANT & FOOD INSPECTION CENT OF TIANJIN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
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AI Technical Summary

Problems solved by technology

In order to avoid this situation, many scholars have improved by adding adsorption materials during the extraction process, such as using styrene-divinylbenzene extraction sheets and activated carbon fibers, etc., but these adsorption materials often need to cool down before decomposing. At this time, the extraction target will also be redistributed, so how to avoid redistribution after extraction is the key to the application of superheated liquid water extraction technology

Method used

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  • Dynamic superheated liquid water extraction device and method for veterinany drug residues in food

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Experimental program
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Effect test

Embodiment 1

[0029] Embodiment 1: Dynamic superheated liquid water extraction of organochlorine pesticides in Poria cocos

[0030] Pulverize the Poria cocos sample, grind and sieve (80 mesh), weigh about 0.2g of the sample powder, add 0.1mg / kg of 12 kinds of organic chlorine mixed standards, and mix it with 0.5g of sea sand (60-100 mesh) after standing overnight , into an extraction pool with an inner diameter of 4.6mm, and extract with superheated liquid water, the flow rate of the liquid delivery pump 1 is 0.5mL / min, the extraction temperature is 120°C, and the extraction time is 60min. After the extraction is completed, elute with 10 mL of acetonitrile, salt out with sodium chloride, take half of the supernatant and blow it to dryness with nitrogen, redissolve with 200 μL of acetone, filter with a 0.22 μm membrane, and detect with gas chromatography. The test results are shown in Table 1.

[0031] Table 1: Add 0.1mg / kg 12 kinds of organochlorine standard dynamic superheated liquid wate...

Embodiment 2

[0034] Embodiment 2: the dynamic superheated liquid water extraction of quinolones in meat

[0035]Weigh about 2g of the homogenized chicken sample (accurate to 0.01g), add 0.1mg / kg of the mixed standard of 8 kinds of quinolone drugs, mix it with 10g sea sand (60-100 mesh) after the absorption is complete, and put it into the inner diameter The extraction tank is 10mm, and the insufficient part is filled with sea sand. The extraction was performed with superheated liquid water, the flow rate of the liquid delivery pump 1 was set at 1.0 mL / min, the extraction temperature was 120° C., and the extraction time was 60 min. After the extraction was completed, it was eluted with 10 mL of methanol, blown to near dryness with nitrogen, reconstituted with 2 mL of acetonitrile / water (10:90, v / v), filtered through a 0.22 μm membrane, and detected by liquid chromatography. The detection results are shown in Table 2.

[0036] Table 2: The recovery result (%, n=6) of the dynamic superheated...

Embodiment 3

[0039] Example 3: Dynamic superheated liquid water extraction of 20 pesticides in carrots

[0040] Chop the carrots, weigh about 2g (accurate to 0.01g) of the sample, add 0.05mg / kg of a mixed standard of 20 pesticides, mix it with 10g of sea sand (60-120 mesh) after the absorption is complete, and fill the mixture into the inner diameter It is a 10mm extraction pool, and the insufficient part is filled with sea sand. The extraction was performed with superheated liquid water, the flow rate of the liquid delivery pump 1 was set at 1.0 mL / min, the extraction temperature was 110° C., and the extraction time was 60 min. After the extraction is completed, elute with 10 mL of acetonitrile, salt out and separate layers with sodium chloride, take half of the supernatant, blow it to dryness with nitrogen, redissolve with 1 mL of acetone, pass through a 0.22 μm organic filter membrane, and detect by gas chromatography-mass spectrometry. The results are shown in Table 3.

[0041] Table...

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Abstract

The invention relates to a dynamic superheated liquid water extraction device and a method for veterinany drug residues in food. The device comprises a liquid delivery pump, a temperature control cabinet, an extraction pond and an adsorption pipe, wherein a stainless steel preheating coil and the extraction pond are arranged in the temperature control cabinet. The adsorption pipe, the extraction pond and the liquid delivery pump are connected through a switching valve and are switched according to an operation requirement. According to the method, the superheated liquid water extraction is combined with a C18 padding solid phase adsorption technology, so that the extraction efficiency is increased, the operation steps are simplified and different sizes of the extraction pond and padding elution modes can be selected according to the difference in food classification. The method is a new technology for extracting the veterinany drug residues in food, with high efficiency, low consumption, environmental protection and excellent application prospect.

Description

technical field [0001] The invention relates to an extraction device and method for residual agricultural and veterinary drugs in food, in particular to a dynamic super-hot water extraction device and method for residual agricultural and veterinary drugs in food, belonging to the field of food detection. Background technique [0002] Sample pretreatment technology is one of the most critical steps in food analysis and testing. The content of target compounds in food samples is generally very small, the matrix is ​​complex, and there are many interferences. Improper pretreatment process often leads to lengthy detection cycle, increased reagent consumption, and even failure of final analysis and detection. Therefore, the research on sample pretreatment technology should be strengthened. , improving the extraction efficiency of residual pesticides and veterinary drugs in food samples, and reducing the amount of toxic reagents are of great significance for ensuring the country's...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/02B01D15/00G01N30/06G01N30/08
Inventor 林安清宓捷波孙祥丽
Owner ANIMAL & PLANT & FOOD INSPECTION CENT OF TIANJIN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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