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Method for rapidly determining sulfonamide antibiotics in water through full-automatic online extraction and ultra-high performance liquid chromatography-tandem mass spectrometry

A technology of high performance liquid chromatography and sulfonamides, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of long pretreatment and analysis and test time, heavy workload, etc., achieve rapid determination, reduce errors, and improve detection sensitivity Effect

Active Publication Date: 2021-07-23
JIANGNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above-mentioned pretreatment methods all require manual extraction experiments, the workload is relatively large, and the time for pretreatment and analysis and testing is relatively long.

Method used

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  • Method for rapidly determining sulfonamide antibiotics in water through full-automatic online extraction and ultra-high performance liquid chromatography-tandem mass spectrometry
  • Method for rapidly determining sulfonamide antibiotics in water through full-automatic online extraction and ultra-high performance liquid chromatography-tandem mass spectrometry
  • Method for rapidly determining sulfonamide antibiotics in water through full-automatic online extraction and ultra-high performance liquid chromatography-tandem mass spectrometry

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Experimental program
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Effect test

Embodiment 1

[0044] (1) Reagent configuration:

[0045] Formic acid: 98% formic acid

[0046] Mobile phase A: ultrapure aqueous solution containing 1% formic acid

[0047] Mobile phase B: methanol with 1% formic acid

[0048] Mobile phase C: methanol / acetone / n-hexane (volume ratio 1:1:1)

[0049] mobile phase A 1 : Ultrapure aqueous solution containing 0.1% formic acid

[0050] mobile phase B 1 : Acetonitrile solution.

[0051] (2) Sample processing:

[0052] (1) Take the water sample and filter it through a polyvinylidene fluoride membrane with a pore size of 0.22 μm. If the water sample has many particles, you can first centrifuge it at 6000rmp for 10 minutes, take the supernatant and filter it through the filter to remove the particles.

[0053] (2) Add formic acid to adjust the pH value, adjust the pH value to 2-3, and put it into a sample bottle for testing.

[0054] (3) Online extraction pretreatment conditions:

[0055] The online pre-extraction treatment equipment used con...

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Abstract

The invention discloses a method for rapidly determining sulfonamide antibiotics in water through full-automatic online extraction and ultra-high performance liquid chromatography-tandem mass spectrometry, and belongs to the technical field of analysis and detection. According to the method, specific full-automatic on-line solid-phase extraction conditions are matched with specific ultra-high performance liquid chromatography-tandem mass spectrometry conditions, so that sample enrichment, purification, separation and determination are realized, and 15 sulfonamide antibiotics in water are analyzed in a full-automatic manner. The method is convenient, efficient and rapid, all analysis steps are automatically completed by an instrument only after a sample is filtered, full-automatic operation is achieved, the whole determination time is only 17 min, the detection limit reaches the ng / L level, the common matrix effect problem in complex matrix sample analysis is solved in the mode of purifying an online solid-phase small column through methanol / pure water, and the ultra-trace detection requirement of the sulfonamide antibiotics in the water is met.

Description

technical field [0001] The invention specifically relates to a method for the rapid determination of sulfonamide antibiotics in water by fully automatic online extraction ultra-high performance liquid chromatography tandem mass spectrometry, which belongs to the technical field of analysis and detection. Background technique [0002] Since penicillin was discovered and used clinically in 1929, more than a hundred antibiotics have been developed and utilized, and they have played a huge role in the treatment of infectious diseases, effectively safeguarding human life and health. In addition, antibiotics are also widely used in animal husbandry and aquaculture to prevent and control infectious diseases, and as antibacterial growth promoters to accelerate the growth of animals. According to their structure and properties, antibiotics can be divided into sulfonamides, quinolones, macrolides, β-lactams, aminoglycosides, tetracyclines, polypeptides, chloramphenicol and other antib...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08G01N30/30G01N30/32G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/08G01N30/30G01N30/32G01N30/34G01N30/72G01N30/8675G01N2030/062G01N2030/324
Inventor 沈斐刘奇欣许燕娟沈明任敏章嘉晴魏竹秋王硕李激
Owner JIANGNAN UNIV
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