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Method and liquid mass database for detecting residual chemicals in animal-derived food

A technology for detecting animals and animal sources, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems that the detection and verification rules of various types of residues are not yet perfect, lack of matrix standard data, and residue forms are different.

Active Publication Date: 2015-09-23
INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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), and the multi-type residue detection and verification rules have not yet been perfected;
[0005] (3) The blank matrix required for method development is difficult to obtain, and the preparation of mixed standard solutions is difficult;
[0007] 1) Only MS / MS data, no chromatographic system information characteristics;
[0008] 2) No online information feature;
[0009] 3) There is no unified pretreatment method coupled with instrumental analysis;
[0010] 4) Lack of matrix standard data
[0011] Therefore, under the existing conditions, it is difficult to effectively realize the rapid screening analysis of multiple types of residues based on liquid mass spectrometry library technology.

Method used

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  • Method and liquid mass database for detecting residual chemicals in animal-derived food
  • Method and liquid mass database for detecting residual chemicals in animal-derived food
  • Method and liquid mass database for detecting residual chemicals in animal-derived food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0092] Embodiment 1. Preparation of standard working solution

[0093] Steroid hormone compounds, nitroimidazole drugs and their metabolites, and Beta-receptor agonist substances: use acetonitrile to prepare their mixed standard stock solutions (0.01g / L), and the substance standard stock solutions can be stable for 12 moon.

[0094] Dyestuffs and other substances are classified into methanol to prepare their mixed standard stock solution (0.01g / L), which can be stable for 3 months.

[0095] Mix and standard working solution (0.1mg / L), respectively pipette testosterone, prednisolone, betamethasone, dexamethasone, metronidazole, ronidazole, dimetridazole, clenbuterol, Appropriate amount of buterol, cimaterol, crystal violet and leuco crystal violet standard stock solutions are used, and a mixed standard solution with a concentration of 0.1mg / L is prepared with acetonitrile. The solution is stable at -20°C for 1 month.

Embodiment 2

[0096] Embodiment 2. Analysis pretreatment method

[0097] The 12 target compounds (Group A substances) belong to 4 compound categories, including steroid hormones, nitroimidazoles, β-receptor agonists and dyes, and their implementation limit requirements range from 0.05 μg / kg to 0.8 μg / kg is a group of drugs with the most stringent limit requirements in the world. Therefore, the steps of purification and concentration were considered in the design of the pretreatment process to meet the strict limit requirements. Aiming at the types of compounds involved in Group A substances, the extraction and purification technology of rapid enzymatic hydrolysis (release of bound state residues) + rapid solid phase extraction (SPE) was designed, which can quickly and effectively complete the pretreatment process of 12 ultra-low limit substances . The specific extraction and purification process is as follows:

[0098] (1) Extraction: Weigh 5g of homogeneous sample (accurate to 0.01g) an...

Embodiment 3

[0103] Embodiment 3. Research on one-time sampling chromatographic analysis system

[0104] 1. Selection of chromatographic column

[0105] 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 residual chemicals in animal-derived food and an application method of the liquid mass database. The production method of the liquid mass database includes the steps of firstly, preparing standard solution; secondly, using the extraction purification technology combining fast enzymolysis and fast solid-phase extraction (SPE) to preprocess a to-be-detected sample before analysis; thirdly, performing one-step sample chromatographic analysis; fourthly, building the liquid mass spectrum database.

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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