Method and liquid mass database for detecting chemical residues in animal-derived food

A technology for detecting animals and animal sources, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the limit requirements and use regulations, there is no unified pretreatment method coupled with instrument analysis, and multi-type residue detection verification rules Issues not yet perfect

Active Publication Date: 2015-09-02
INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

However, whether in terms of method development, validation and standardization, or the improvement of regulations, there are many difficulties in the simultaneous detection of multiple types of residues:
[0003] (1) The chemical properties of different types of veterinary drugs are very different, the polar coverage is wide, and the residue forms in different matrices are different. Individual veterinary drugs still need derivatization to be effectively detected. It is difficult to achieve an effective breakthrough;
[0004] (2) The regulations have different limit requirements and use regulations for different veterinary drugs (banned drugs and restricted drugs), ...

Method used

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  • Method and liquid mass database for detecting chemical residues in animal-derived food
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  • Method and liquid mass database for detecting chemical residues in animal-derived food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0109] Embodiment 1. Preparation of standard working solution

[0110] Mixed standard working solution of 99 substances (0.5mg / L): Pipette 0.5mL of each of the above mixed standard stock solutions (except the mixed standard stock solution of nitrofuran metabolites and their 2-nitrobenzaldehyde derivatives) into a 10mL volumetric flask , dilute to the mark with acetonitrile, and mix well. The solution is stable at -20°C for 1 month;

[0111] Mixed standard working solution of 101 substances (0.5mg / L): Pipette 0.5mL of each of the above mixed standard stock solutions (except the mixed standard stock solution of nitrofuran metabolites) into a 10mL volumetric flask, dilute to the mark with acetonitrile, and mix uniform, the solution is stable at -20°C for 1 month;

[0112] Mixed standard working solution of nitrofuran metabolites (0.5mg / L): pipette 0.5mL of mixed standard stock solution of nitrofuran metabolites into a 10mL volumetric flask, dilute to the mark with acetonitrile, ...

Embodiment 2

[0113] Embodiment 2. Analysis pretreatment method

[0114] For the pretreatment optimization of 103 target compounds (group B substances), the concept of the experimental design is as follows: (1) the simpler the pretreatment process, the better; (2) choose a broad extraction solvent; (3) reduce the solvent dosage, while avoiding the loss of target analytes caused by solvent conversion as much as possible; secondly, the analysis of target analytes and matrix is ​​as follows: (1) Hormone substances and β-receptor agonist substances in target analytes need to be released by enzymatic hydrolysis Bound state residual drugs; (2) The determination of nitrofuran metabolites requires acid hydrolysis and derivatization processes; (3) The types of sample matrices selected are quite different, including solid animal tissues (such as muscle) and liquid animal-derived products (milk); (4) There are prohibited substances and restricted substances in the target analyte.

[0115] The specifi...

Embodiment 3

[0127] Embodiment 3. Research on one-time sampling chromatographic analysis system

[0128] 1. Selection of chromatographic column

[0129] Ultrafine particle (particle size <2 μm) chromatographic columns are usually considered for liquid chromatographic separation of multi-target analytes. However, this study uses a conventional HPLC system with a pressure upper limit of 400 Bar, so ultra-high performance liquid chromatography columns cannot be used. In order to achieve the separation purpose of the design, considering the system pressure limitation, the particle size range of the chromatographic column is controlled between 2 μm and 3 μm, and the length of the chromatographic column is 100 mm to 150 mm; In terms of chromatographic column type, a C18 chromatographic column suitable for separating a wide polarity range was selected. Through the above limitations, this study selected one of each type of compound based on polarity (selected with reference to the LogD value), an...

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Abstract

The invention relates to a liquid mass database for detecting chemical residues in animal-derived food and a using method thereof. The method for establishing the database comprises the following steps that 1, a standard working solution is prepared; 2, treatment before analysis is conducted, wherein treatment before analysis is conducted on a sample to be tested according to the extraction and purification technique based on rapid enzymolysis and rapid solid-phase extraction (SPE); 3, chromatographic analysis is conducted at a time; 4, a liquid mass spectrogram library is established.

Description

technical field [0001] The invention belongs to the field of biological detection, and in particular relates to a liquid-mass database for detecting residual drugs in animal-source food and a method for using the same. Background technique [0002] Foods of animal origin account for a considerable proportion of international trade in agricultural products, and regulations and restrictions on drug residues in foods of animal origin are becoming more and more stringent. Taking Japan’s “Positive List” system implemented in May 2006 as an example, 236 types of veterinary drugs and feedstuffs Additives have set specific limit standards, and in the field of domestic food safety, from the early "chloramphenicol, nitrofuran" to the later "malachite green, clenbuterol", frequent food safety incidents caused by drug residues have become prominent The technical support capability of my country's food safety supervision and control system is insufficient, and it is urgent to establish a r...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 张鸿伟张晓梅梁成珠
Owner INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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