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Method for synchronously detecting residual quantity of various antibiotics in pig raising wastewater

A technology of simultaneous detection and antibiotics, applied in the field of trace environmental pollutant detection, can solve the problems of single type of antibiotic detection, large amount of water samples to be detected, poor anti-interference ability, etc., to reduce pretreatment time, strong anti-interference ability, The effect of low detection limit

Active Publication Date: 2020-10-09
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of single type of antibiotic detection, large amount of water sample, high detection limit and poor anti-interference ability in the existing detection method, the present invention provides a A method for simultaneous detection of multi-type antibiotic residues in swine wastewater

Method used

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  • Method for synchronously detecting residual quantity of various antibiotics in pig raising wastewater
  • Method for synchronously detecting residual quantity of various antibiotics in pig raising wastewater
  • Method for synchronously detecting residual quantity of various antibiotics in pig raising wastewater

Examples

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Embodiment 1

[0039] Pig wastewater was collected in three batches from a pig farm in Harbin, and the residual amount of antibiotics in the wastewater was detected by the following method.

[0040] Detection method:

[0041] (1) Sample pre-treatment: Collect swine wastewater samples, centrifuge at 8000r / min for 5min, and pass the supernatant through a 0.7μm microporous membrane. Subsequently, accurately draw 40mL of the filtrate and dilute it to 200mL with ultrapure water, and accurately add 0.1gNa 2After EDTA, adjust the pH to 2 with 6mol / L hydrochloric acid solution. Then, the Oasis HLB column with a specification of 6cc / 200mg was used to enrich and purify the water sample. Before use, the HLB column needs to be activated with 5mL methanol and 10mL ultrapure water in sequence, and the activation is repeated 3 times. Then the water sample was passed through the HLB column under the action of gravity flow, and the flow rate of the column was controlled at about 1 mL / min. After the water ...

Embodiment 2

[0055] This embodiment is the establishment process of liquid chromatography detection conditions.

[0056] (1) Selection of liquid chromatography mobile phase

[0057] Methanol and acetonitrile are organic solvents commonly used in reversed-phase chromatography. The volume ratios of methanol and acetonitrile in the present invention are respectively 100:0, 80:20, 80:20, 70:30, 60:40, 50:50, 40:60 , 30:70, 20:80 and 0:100, the separation effect of the chromatographic peaks of 10 antibiotics to be tested. It was found that with the increase of the proportion of acetonitrile in the organic phase, the resolution of the chromatographic peaks of the 10 antibiotics gradually increased. Therefore, pure acetonitrile was chosen as the organic phase.

[0058] Then, with acetonitrile as the organic phase, 0.1% formic acid, 0.2% formic acid, 0.3% formic acid, 0.4% formic acid, 5mmol / L ammonium acetate, 67mmol / L phosphoric acid, 67mmol / L ammonium dihydrogen phosphate, 50mmol / L citric a...

Embodiment 3

[0067] This embodiment is the establishment process of mass spectrometry conditions. Due to its high sensitivity, the electrospray ion source chooses the positive ion mode to monitor the target antibiotics. Protonated Adducts of Molecular Ions [M+H] + Used to quantify the precursor ions (parent ions) of each antibiotic. Antibiotics were made into 1mg / L standard solutions as tuning solutions, and the Intellistart function of Masslynx software was used for automatic tuning to optimize the conical voltage, monitoring ion pairs and collision energy of various antibiotics, and select the one with high response and stability. Product ions (product ions) are used as quantitative ions, and product ions with lower response are qualitative ions for monitoring in MRM mode. The mass spectrometry parameters related to the target antibiotic obtained after tuning are shown in Table 1.

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Abstract

The invention discloses a method for rapidly, efficiently and synchronously detecting the residual quantity of various antibiotics in pig raising wastewater, and belongs to the technical field of detection of trace environmental pollutants. The invention solves the problems of single antibiotic detection type, large detection water sample amount, high detection limit, poor anti-interference capability and the like in an existing detection method. The invention provides an analysis method for simultaneously detecting various antibiotics in pig raising wastewater based on a solid-phase extraction-ultra-high performance liquid chromatography tandem mass spectrometry technology through selection of chromatography, mass spectrometry, solid-phase extraction and pretreatment conditions. Accordingto the method, only 40mL of water sample is needed, so that the pretreatment time is greatly shortened; under the standard concentrations of a low level, a medium level and a high level, the recoveryrates of 10 antibiotics are all between 74.1% and 118.2%, and the relative standard deviation is within the range of 0.14% to 11.74%. In addition, the method is low in detection limit and high in anti-interference capability, and the lower detection limit reaches 2.5-10 ng / L.

Description

technical field [0001] The present invention relates to a method for synchronous detection of multi-type antibiotic residues in pig-raising wastewater, in particular to a method for synchronous detection of multi-type antibiotic residues in pig-raising wastewater by using solid-phase extraction-ultra-high performance liquid chromatography tandem mass spectrometry technology, It belongs to the detection technology of trace environmental pollutants. Background technique [0002] In order to prevent, treat and promote animal growth, a large amount of antibiotics are used in livestock and poultry farming every year. Among them, tetracyclines, sulfonamides, and fluoroquinolones are the most widely used antibiotics in the swine industry. However, most veterinary antibiotics are only absorbed by the body after ingestion, and most of the drug residues are excreted with feces and urine in the form of prototypes. % to 90%, about 30% to 83.7% of fluoroquinolones are excreted. This m...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06G01N30/08G01N30/72
CPCG01N30/88G01N30/06G01N30/08G01N30/72G01N2030/8809G01N2030/062G01N2030/027G01N2030/085G01N2030/047
Inventor 孟佳田雅婕樊译阳刘敏
Owner HARBIN INST OF TECH
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