Method for simultaneously detecting six types of 24 antibiotics in livestock excrements by combination of ultrasonic extraction-solid phase extraction pretreatment and liquid chromatography-mass spectrometry technology

A livestock and poultry manure, LC-MS technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of limited quantity and recovery rate of antibiotics detected, many interferences, instability, etc., to improve selectivity and enrichment. The effect of multiple times, large adsorption capacity and easy operation

Inactive Publication Date: 2018-04-13
SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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  • Abstract
  • Description
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Problems solved by technology

[0005] The purpose of the present invention is to overcome the problems of instability, high interference, limited quantity and recovery rate of antibiotics in the existing method, and provide a method with accurate and stable detection results, less interference, fast and efficient detection process, using ultrasonic Extraction, HLB solid phase extraction column purification pretreatment combined with liquid chromatography tandem mass spectrometry (LC-MS / MS) can simultaneously determine six types (sulfonamides, tetracyclines) in livestock and poultry manure (chicken manure, cow manure, pig manure, etc.) , fluoroquinolones, macrolides, amide alcohols and penicillins) 24 antibiotics with different structures (the 24 antibiotics are sulfamethoxazole, sulfadiazine, sulfachloropyridazine, sulfamethoxine, sulfadimethoxine Meisoxazole, sulfadimethoxine, sulfamethazine, azithromycin, clarithromycin, erythromycin, spiramycin, tilmicosin, ciprofloxacin hydrochloride, fleroxacin, ofloxacin Star, enrofloxacin, oxytetracycline hydrochloride, chlortetracycline hydrochloride, amoxicillin trihydrate, penicillin G methyl salt, thiamphenicol, fluthiamphenicol, chloramphenicol, chlorhexidine hydrochloride ) method, that is, a method for the simultaneous detection of six types of 24 antibiotics in livestock and poultry feces by ultrasonic extraction-solid phase extraction pretreatment combined with liquid chromatography-mass spectrometry

Method used

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  • Method for simultaneously detecting six types of 24 antibiotics in livestock excrements by combination of ultrasonic extraction-solid phase extraction pretreatment and liquid chromatography-mass spectrometry technology
  • Method for simultaneously detecting six types of 24 antibiotics in livestock excrements by combination of ultrasonic extraction-solid phase extraction pretreatment and liquid chromatography-mass spectrometry technology
  • Method for simultaneously detecting six types of 24 antibiotics in livestock excrements by combination of ultrasonic extraction-solid phase extraction pretreatment and liquid chromatography-mass spectrometry technology

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Effect test

Embodiment 1

[0044] Embodiment 1: standard addition recovery experiment

[0045] The invention adopts an internal standard method to determine the influence of the pretreatment method on the recovery rate of six types of 24 kinds of antibiotics in livestock and poultry manure. The standard addition recovery experiment is divided into low-level addition and high-level addition two kinds: low-level addition is to add 0.2mL 10mg / L mixed standard solution (mixed standard solution is to contain 24 kinds of antibiotics) respectively in three kinds of feces mixed standard solution); the high-level addition amount is to add 2mL of 10mg / L mixed standard solution to the three types of feces respectively. Specifically follow the steps below:

[0046] Step 1. Extraction of livestock and poultry manure

[0047] The collected fresh chicken manure, cow manure and pig manure were respectively freeze-dried, crushed and passed through a 0.25mm sieve. Three sets of samples were set up for each type of fec...

Embodiment 2-3

[0080] Example 2-3: Determination of antibiotic content in actual stool samples

[0081] Collect the feces (chicken manure, pig manure and cow manure) of a chicken farm, pig farm and dairy farm in Shanghai, first adopt the method (ultrasonic extraction) of step 1 of the present invention to carry out sample pretreatment, and then use the solid phase of step 2 of the present invention The extraction method is pre-treatment for enrichment and purification, and then the actual concentration of the sample is detected and analyzed by the liquid chromatography-mass spectrometry detection method in step 3 of the present invention. The specific detection process is as follows:

[0082] (1) Extraction of livestock and poultry manure samples

[0083] The collected fresh chicken manure, cow manure and pig manure were respectively freeze-dried, crushed and passed through a 0.25mm sieve. Accurately weigh 1.000 g of each stool sample into a 30 mL glass centrifuge tube. Add 10 μL of 5 mg / ...

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Abstract

The invention discloses a method for simultaneously detecting six types of 24 antibiotics in livestock excrements by combination of ultrasonic extraction-solid phase extraction pretreatment and a liquid chromatography-mass spectrometry technology. The method comprises the following steps: (1) adding an internal standard substance for indicating the recycling rate in advance, and performing ultrasonic extraction; (2) performing solid phase extraction to enrich and purify target antibiotics; (3) performing the liquid chromatography-mass spectrometry technology to detect the contents of the 24 antibiotics. According to the method, the residue conditions of the six types of 24 antibiotics in the livestock excrements can be simultaneously detected at one time; the time of the detection processis short, the detection precision is high, the sensitivity, the stability and the selectivity are high, and the detection limit is low; by optimization of an extraction solvent, chelation between theantibiotics and metal ions in the excrements can be effectively reduced, so that the target antibiotics are separated from a sample, and the recycling rate is increased; furthermore, the method is easy and convenient to operate, high in enrichment factor and high in repetitiveness. The internal standard substance for indicating the recycling rate is added before the whole pretreatment process, sothat the loss of target substances in the pretreatment process can be well expressed, and a final result is more real and reliable.

Description

technical field [0001] The invention belongs to the technical field of detection of trace organic pollutant residues in livestock and poultry manure, relates to a method for detecting antibiotics in livestock and poultry manure, in particular to a combination of ultrasonic extraction-solid phase extraction pretreatment combined with liquid chromatography tandem mass spectrometry ( LC-MS / MS, referred to as liquid mass spectrometry), can efficiently process and simultaneously detect six types of up to 24 kinds of antibiotic substances in livestock and poultry manure (chicken manure, cow manure, pig manure). technical background [0002] With the development of modernization, scale and intensification of the livestock and poultry breeding industry, antibiotics are widely used in the livestock and poultry breeding process. However, most antibiotics cannot be fully absorbed, and about 40%-90% of them are excreted from the animal body in the form of parent or metabolites, enter th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08G01N30/88
CPCG01N30/08G01N30/88
Inventor 胡双庆沈根祥张洪昌钱晓雍王振旗朱英张玉袁哲军
Owner SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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