Liquid chromatography-mass spectrometry detection method for cephalosporin antibiotics

A liquid chromatography and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of improving the experimental recovery rate, improving the recovery rate, and good specificity

Inactive Publication Date: 2020-08-14
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is exactly in order to overcome the defect that above-mentioned prior art exists and provide a kind of liquid chromatography-mass spectrometry that solves ...

Method used

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  • Liquid chromatography-mass spectrometry detection method for cephalosporin antibiotics
  • Liquid chromatography-mass spectrometry detection method for cephalosporin antibiotics
  • Liquid chromatography-mass spectrometry detection method for cephalosporin antibiotics

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] 1. Preparation of standard solution:

[0052] Weigh 10mg of standard samples respectively, put them in beakers, and dissolve them with 100ml of methanol to prepare 10mg / L standard solutions, and store them at -20°C. Prepare mixed standards of different concentrations according to the required concentration.

[0053] 2. Sample pretreatment

[0054]Take 1 L of water samples containing cephalexin, cephradine, cefaclor, cefuroxime, and cefotaxime from the sewage treatment plant, remove suspended solids through a centrifuge, and filter the water samples through a 0.222 μm glass fiber filter membrane after centrifugation. Add 0.5M HCL to adjust the pH of the water sample to 2.5. Add 20ml Na 2 EDTA and mix well. The water sample was extracted through the HLB extraction column. First rinse the extraction column with 10ml methanol and 10ml ultrapure water for activation. The water sample passed through the extraction column at a flow rate of 5ml / min. The column after samp...

Embodiment 2

[0061] The difference from Example 1 is that 0.5M HCL is added to adjust the pH of the water sample to 1.5.

Embodiment 3

[0063] The difference from Example 1 is that 0.5M HCL is added to adjust the pH of the water sample to 3.5.

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Abstract

The invention relates to a liquid chromatography-mass spectrometry detection method of cephalosporin antibiotics. The method is characterized by comprising the following steps: (1), performing samplepretreatment; to be specific, removing suspended matters from a certain number of water sample through a centrifuge, carrying out suction filtration, and regulating the pH value of the water sample; (2), performing sample extraction; to be specific, leaching an extraction column for activation, then adding a chelating agent into the water sample and fully mixing the substances, enabling the watersample to pass through an extraction column, then flushing the sample-passing extraction column, then performing drying and eluting, collecting eluent and blowing the eluent to be nearly dry to obtainresidues; and (3), performing mass spectrum detection; to be specific, dissolving the residues to obtain a to-be-detected solution, and detecting the to-be-detected solution under certain gradient elution conditions and mass spectrum detection conditions. Compared with the prior art, the method has the advantages of simple operation, strong specificity, high accuracy, good tolerance, high instrument sensitivity and the like.

Description

technical field [0001] The invention relates to the field of environmental analysis, in particular to a liquid chromatography-mass spectrometry detection method for cephalosporin antibiotics. Background technique [0002] Liquid chromatography-mass spectrometry is a combination of two techniques, which combines high-efficiency separation and structure identification, and becomes a powerful tool for the identification and quantification of trace components in complex mixtures. [0003] Liquid chromatography uses liquid as the mobile phase, which is especially suitable for the analysis of high-boiling macromolecules, strong polarity and poor thermal stability compounds, and is more suitable for the analysis of many drugs, such as tetracyclines with thermal instability. The development of science and technology in the past few decades has promoted the development of liquid chromatography-mass spectrometry technology. Liquid chromatography-mass spectrometry is the combination of...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/34G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/34G01N30/72G01N2030/062G01N2030/146
Inventor 王娟程恒友毕东苏刘静董璇璇朱艺文
Owner SHANGHAI INST OF TECH
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