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Fast high-precision detecting method for animal medicine residue in food

A technology for veterinary drug residues and detection methods, applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of high requirements for experimental skills, cumbersome data processing, heavy workload, etc., to improve the efficiency of analysis and detection, shorten the pre-processing time, The effect of reducing the cost of experiments

Inactive Publication Date: 2008-08-20
CHINESE ACAD OF INSPECTION & QUARANTINE
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Problems solved by technology

At present, GC-MS (gas chromatography-mass spectrometry) technology is the most commonly used method at home and abroad to analyze the residues of pesticides and veterinary drugs, but most of these methods have insufficient detection sensitivity, or the pretreatment steps are cumbersome and time-consuming: such as the national standard method, the Japanese notification method, etc. For example, the method of pretreatment including multi-step liquid-liquid distribution and decompression concentration process takes about 5-6 hours to complete the whole pretreatment process; or the analysis cost is high, which cannot meet the requirements of rapid and accurate determination of various foods: if known The post-data processing method of using the matrix-matched standard solution as the standard working solution to draw the standard curve. Every time a matrix is ​​analyzed, the standard curve of the matrix must be prepared again. For those who need to complete the detection tasks of pesticide residues in a large number of different matrices It is said that the workload is huge, the requirements for experimental skills are high, and the data processing is cumbersome, which cannot meet the rapid and multi-residue analysis and detection requirements of front-line experimenters (such as import and export commodity inspection departments).

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  • Fast high-precision detecting method for animal medicine residue in food
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Experimental program
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Effect test

Embodiment 1

[0017] Embodiment 1: the detection method and the result of the method of the present invention to apple matrix:

[0018] (1) Method steps:

[0019] Weigh 20 g of apples, add 50 mL of acetonitrile, homogenize with a high-speed tissue homogenizer at 9500 r / min, extract for 2 minutes, and then filter with suction. The two obtained solutions were combined, and the volume was adjusted to 100 mL with acetonitrile to be purified. Take 1mL extract solution through C 18 (30mg) column, elute with 1mL80% acetonitrile / water solution, collect all effluents, add 2mL water to it and pass C 18 (50 mg) column. After adding 20% ​​NaCl aqueous solution 20mL to the effluent, pass through the above C again 18 (50 mg) column and discard the effluent. Suction filter and dry the C18 (50mg) column for 2min, then connect to the GCS (30mg) / PSA (30mg) column, elute with 1mL toluene / acetone / n-hexane (1 / 3 / 6) mixed solution, add Prepared analytical protectant solution 20 μ L, described analytical pro...

Embodiment 2

[0034] Embodiment 2: the comparison experiment result of method of the present invention and matrix matching standard solution correction method

[0035] Using this method and the matrix-matching standard solution calibration method, 40 pesticides in mushroom and cabbage blank matrices were quantitatively determined, wherein the method of the present invention was the same as in Example 1, and the added concentration of pesticides was 50 μg / kg. Figure 1 shows the quantitative results of some pesticides. It can be seen from Figure 1 that using the standard solution added with analytical protective agent as the working curve can basically accurately quantify the residual pesticides in the matrix, compensate for the influence of the matrix effect on the quantitative results, and can replace the original matrix matching standard solution calibration method. When performing pesticide residue detection on different crops, it is no longer necessary to make a matrix-matched standard s...

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Abstract

The invention provides a fast high-accuracy method for detecting agricultural and veterinary products residues in food, including following four steps: (1) matrix pre-treatment; (2) adding analysis protecting agent; (3) introducing sample and detecting on machine; (4) data processing. The detecting method, under the condition that GC / MS instrument detecting sensitivity is no changed, and with large volume injection, could reduce pre-treatment sample amount sharply. At the same time the invention has the advantages of low analysis cost, short analysis time, and uses the standard solution containing analysis protecting agent as standard working solution to draw standard curve for quantifying agricultural and veterinary products residues in various kinds of vegetable, fruit and corn substrates, and quantifies agricultural and veterinary products residues in various kinds of substrates with one standard curve, and has good applicability, the sensibility, accuracy and precision are all in accordance with command of agricultural and veterinary products multi-residues technology, and is suitable for detecting various kinds of agricultural and veterinary products' residues in food quickly and sensitively.

Description

technical field [0001] The invention relates to a fast and high-precision detection method for agricultural and veterinary drug residues in food. Background technique [0002] At present, with the wide application of agricultural and veterinary drugs, while increasing the output of agricultural products, the impact of their residues on human health has also attracted more and more attention. In the "Positive List System of Agrochemical Residues in Food" implemented in Japan in June, the residue limit value of most agricultural and veterinary drugs is 10 μg / kg. At present, GC-MS (gas chromatography-mass spectrometry) technology is the most commonly used method at home and abroad to analyze the residues of pesticides and veterinary drugs, but most of these methods have insufficient detection sensitivity, or the pretreatment steps are cumbersome and time-consuming: such as the national standard method, the Japanese notification method, etc. For example, the method of pretreatm...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 李翔李礼许秀丽仲维科刘汉霞张垚孙毅之陈彦长
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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