Method for simultaneously analyzing various aminoglycoside compound residues in agricultural and animal products

A technology for aminoglycosides and compounds, applied in the field of simultaneous analysis of residues of various aminoglycoside compounds in agricultural and animal products, can solve problems such as cumbersome operations, incompatibility, and weak retention, and achieve the effect of improving the throughput of detection and analysis

Inactive Publication Date: 2018-09-11
烟台杰科检测服务有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aminoglycoside antibiotics are alkaline and highly polar, and their retention on C18 columns is weak, coupled with the lack of chromogenic and fluorescent groups, it is difficult to detect using conventional methods
Our country currently has no standards for the detection of aminoglycoside compounds in agricultural products. The detection standards for animal foods, such as GB 21323-2007 "Determination of Aminoglycoside Drug Residues in Animal Tissues by High Performance Liquid Chromatography-Mass Spectrometry / Mass Spectrometry", GB / T 22969-2008 "Determination of streptomycin, dihydrostreptomycin and kanamycin residues in milk powder and milk by liquid chromatography-tandem mass spectrometry", GB / T 22945-2008 "Streptomycin in royal jelly Determination of Dihydrostreptomycin and Kanamycin Residues by Liquid Chromatography-Tandem Mass Spectrometry", when detecting aminoglycoside compound residues in food according to the above three standards, ion-pair reagents are used, which is cumbersome and easy to operate. Produces ion suppression effects or is incompatible with mass spectrometry, increasing maintenance costs
[0004] Domestic reports on the simultaneous detection of streptomycin and other aminoglycoside compounds are limited to animal foods, and there is a lack of research on related methods for simultaneous detection in agricultural and animal products

Method used

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  • Method for simultaneously analyzing various aminoglycoside compound residues in agricultural and animal products
  • Method for simultaneously analyzing various aminoglycoside compound residues in agricultural and animal products
  • Method for simultaneously analyzing various aminoglycoside compound residues in agricultural and animal products

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Take the above-mentioned negative fruit and vegetable samples, that is, a mixture made evenly of 13 kinds of fruits and vegetables including apples, kohlrabi, Chinese cabbage, spinach, green stems, potatoes, taro, green beans, carrots, onions, ginger, garlic sprouts, and shallots. Matrix, detect streptomycin and dihydrostreptomycin residual content of two aminoglycoside compounds, the steps are as follows:

[0026] (1) Extraction: Weigh 3.0 g of evenly prepared fruit and vegetable samples into a plastic centrifuge tube, add 15 mL of 0.01 mol / L ammonium acetate buffered saline solution for extraction, vortex and mix well, and centrifuge at 4000 r / min for 5 min; Put the supernatant in another 50mL plastic centrifuge tube, repeat the extraction of the residue once, combine the supernatant into the centrifuge tube, take 10mL of the combined extract and use a pH meter to adjust the pH value to 6.50±0.05: first use 10mol / L hydrogen Sodium oxide solution is roughly adjusted, t...

Embodiment 2

[0040] Take the above-mentioned pig lean meat sample, and detect the residual content of 8 kinds of aminoglycoside compounds, the steps are as follows:

[0041](1) Extraction: Weigh 3.0 g of evenly prepared pig lean meat sample into a plastic centrifuge tube, add 15 mL of 0.01 mol / L ammonium acetate buffered saline solution for extraction, vortex and mix well, and centrifuge at 4000 r / min for 5 min ;Transfer the supernatant to another 50mL plastic centrifuge tube, repeat the extraction of the residue once, combine the supernatant into the centrifuge tube, take 10mL of the combined extract and use a pH meter to adjust the pH value to 6.50±0.05: first use 10mol / L sodium hydroxide solution for rough adjustment, and then use 1mol / L sodium hydroxide and 0.1mol / L sodium hydroxide for fine adjustment, and use 6mol / L hydrochloric acid solution or 0.1mol / L hydrochloric acid solution for callback to obtain an aqueous solution;

[0042] (2) Purification: Add 1 g of diatomaceous earth to...

Embodiment 3

[0057] Take the above-mentioned chicken sample, and detect the residual content of 8 kinds of aminoglycoside compounds, the steps are as follows:

[0058] (1) Extraction: Weigh 3.0g of the uniformly prepared chicken sample into a plastic centrifuge tube, add 15mL of 0.01mol / L ammonium acetate buffered saline solution for extraction, vortex and mix well, and centrifuge at 4000r / min for 5min; Put the supernatant in another 50mL plastic centrifuge tube, repeat the extraction of the residue once, combine the supernatant into the centrifuge tube, take 10mL of the combined extract and use a pH meter to adjust the pH value to 6.50±0.05: first use 10mol / L hydrogen Sodium oxide solution is roughly adjusted, then fine-tuned with 1mol / L sodium hydroxide and 0.1mol / L sodium hydroxide, and the excess is adjusted by using 6mol / L hydrochloric acid solution or 0.1mol / L hydrochloric acid solution to obtain an aqueous solution;

[0059] (2) Purification: Add 1 g of diatomaceous earth to the aqu...

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Abstract

The invention discloses a method for simultaneously analyzing various aminoglycoside compound residues in agricultural and animal products. The method comprises the following steps: weighing a sample;adding an ammonium acetate buffering solution; after carrying out oscillation and extraction, carrying out centrifuging; separating an extracting solution obtained by centrifuging and regulating to asuitable range by utilizing a PH (Potential of Hydrogen) meter; purifying by adopting dispersed solid-phase extraction and a solid-phase extraction small column. Ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS), electrospray ionization (ESI) and multi-reaction monitoring (MRM) scanning modes are adopted. Compared with other similar methods, the method disclosed by the invention has the advantages of simplicity in operation and high sample flux; eight types of aminoglycoside compounds including streptomycin, dihydrostreptomycin, spectinomycin, gentamicin, apramycin, kanamycin, amikacin and neomycin are detected at the same time; the detection efficiency is greatly improved, and rapid qualitative and quantitative detection can be rapidly carried out; the detection limit can completely meet domestic and overseas laws and regulations and limitation requirements, and powerful support is provided for food safety guarantees and import and export of the agricultural and animal products of China.

Description

technical field [0001] The invention belongs to the technical field of food detection methods, in particular to a method for simultaneously analyzing residues of multiple aminoglycoside compounds in agricultural and animal products. Background technique [0002] Aminoglycoside antibiotics are a class of antibiotics containing aminoglycoside bonds. They have a broad antibacterial spectrum and have strong antibacterial activity against aerobic Gram-negative bacilli. Aminoglycoside antibiotics have toxic side effects such as ears and kidneys, and can be absorbed by food for a long time. After entering the body, the human body will develop drug resistance, so its residue detection is becoming more and more important. [0003] Aminoglycoside antibiotics are alkaline and highly polar, and their retention on C18 columns is weak. In addition, they lack chromogenic and fluorescent groups and other characteristics, so it is difficult to detect them by conventional methods. Our countr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 肖桂英张禧庆姜向柯王丹
Owner 烟台杰科检测服务有限公司
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