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A method for analyzing sulfonamides by magnetic solid-phase extraction combined with isotope dimethylation labeling

A dimethylation and isotope technology, applied to the analysis of materials, material separation, instruments, etc., can solve the problems of difficult quantitative analysis and difficult to obtain prices for isotope internal standards, to achieve efficient selective enrichment, improve labeling efficiency, Consumption saving effect

Inactive Publication Date: 2018-12-21
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In LC-MS, it is the simplest and most accurate method to use isotope internal standard for quantitative analysis of the target, but because the isotope internal standard is difficult to obtain and the price is high, it is usually only suitable for the analysis of a small number of targets
However, sulfonamides belong to a large class of substances, and it is difficult to carry out quantitative analysis of these targets simultaneously with the isotope internal standard method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: the analysis of sulfa compound in tap water

[0031] 1) Take 1mL of the water sample to be tested, directly measure the total nitrogen without filtering, and calculate the required labeling reagent CD according to the total nitrogen of the sample 2 The consumption of O, its consumption is 50 times (mol ratio) of total nitrogen;

[0032] 2) Take 200mL of the water sample to be tested and add 20mg of the same amount of magnetic carbon nanomaterials (washed three times with acetonitrile and balanced once with ultrapure water) to the water sample A to be tested and the equal volume (0.1μg / L) of sulfonamide mixed standard solution B In, shaking to complete the adsorption and enrichment of sulfa substances;

[0033] 3) Magnetic separation under an external magnetic field, pour off the residual liquid after adsorption, transfer the magnetic carbon nanomaterials that have been adsorbed to 1.5mL centrifuge tubes, add 0.5mL of 50mM sodium phosphate buffer solution (p...

Embodiment 2

[0037] Embodiment 2: the analysis of sulfa compound in river water

[0038] 1) Take river water with different sections and depths, mix and let stand for 1 hour to make the sediment and water preliminarily separate under the action of gravity, take the supernatant (volume greater than 150mL) and filter it as the water sample to be tested;

[0039] 2) Take 1mL of the filtered water sample to be tested, measure its total nitrogen, and calculate the required labeling reagent CH according to the total nitrogen of the sample. 2 The consumption of O, its consumption is 50 times (mol ratio) of total nitrogen;

[0040] 3) Take 100mL of the filtered water sample to be tested, add the same amount of magnetic carbon nanomaterials 50mg (washed three times with acetonitrile, and balance once with ultrapure water) to the water sample A to be tested and an equal volume (1μg / L) of sulfonamide In the mixed standard solution B, shake to complete the adsorption of sulfa substances;

[0041] 4)...

Embodiment 3

[0045] Example 3: Analysis of sulfa compounds in milk

[0046] 1) Take 10 mL of milk sample into a 50 mL centrifuge tube, add 0.5 g of hydroxylamine hydrochloride, vortex and mix well, add 25 mL of ethyl acetate, cover tightly and shake on a shaker (100 r / min) for 20 min;

[0047] 2) Centrifuge (4000r / min), transfer the supernatant to a rotary evaporator and evaporate to dryness (33°C±2°C);

[0048] 3) Dissolve the residue with 10mL of 1% phosphoric acid solution, add 5mL of n-hexane, vortex mix for 2min, let it stand for 10min, remove the n-hexane layer and transfer to a rotary evaporator to evaporate to dryness;

[0049] 4) Redissolve the residue after evaporation to dryness with 10mL 20% methanol solution, as sample A to be tested;

[0050] 5) Take 0.1 mL of sample A, dilute it to 1 mL with water, measure its total nitrogen, and then convert it to obtain the total nitrogen in sample A. According to the total nitrogen in sample A, calculate the required labeling reagent CH...

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Abstract

The invention provides a method for analyzing sulfonamide substances by magnetic solid-phase extraction and isotope dimethyl mark. The method includes the steps: taking magnetic carbon nano-particles as extraction materials; dispersing the materials in sample solution with sulfanilamide; enriching sulfonamide compounds in samples to the surfaces of the magnetic carbon nano-particles by the aid of a solid-phase extraction method; performing dimethyl mark for sulfonamide compound normal positions adsorbing on the surfaces of the materials; eluting and collecting marked samples; analyzing the eluted and collected samples by the aid of an LC-MS (liquid chromatography-mass spectrometry) to obtain results. The new method has the advantages that trace sulfonamide compounds in water are quantitatively analyzed on magnetic nano-spheres by a dimethyl mark method and the LC-MS, the method is simple and convenient to operate, rapid in analyzing, and trace sulfonamide substances in environmental media can be accurately and quantitatively analyzed.

Description

technical field [0001] The invention relates to a new method for qualitative and quantitative analysis of sulfonamide compounds. The method is mainly based on in-situ stable isotope dimethylation labeling of sulfonamide compounds adsorbed on the surface of a magnetic ball, so that each sulfonamide compound has a corresponding isotope Internal standard, to achieve accurate identification and quantification of all sulfonamide targets by LC-MS. Background technique [0002] Sulfonamide compounds are a general term for a class of compounds containing p-aminobenzenesulfonamide structure, and are the earliest synthetic antibacterial drugs. Because the drug has many advantages such as broad antibacterial spectrum, low price, and stable properties, the drug is widely used in both clinical and veterinary medicine fields. However, due to the non-standard use of sulfa drugs in the process of prevention and treatment, many animal-derived foods often have residues of such drugs. Sulfon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 吴明火粟靖云占敬敬胡玉峰龚勋
Owner DALIAN UNIV OF TECH
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