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Method for determining antibiotics in water by solid-phase extraction-liquid chromatography-tandem mass spectrometry by using special column for large-volume water sample

A technology of liquid chromatography and tandem mass spectrometry, which is applied to the field of determination of antibiotics in water with a special column for large-volume water samples, solid-phase extraction-liquid chromatography-tandem mass spectrometry, can solve the problems of time-consuming and other problems, and achieve the effect of a fast and reliable experimental method

Inactive Publication Date: 2019-11-29
福建浩得实验室系统科技有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Most of the existing pretreatments for antibiotics in water use solid-phase extraction column enrichment, and then use LC-MS or LC-MS / MS to achieve the qualitative and quantitative analysis of the target. However, the conventional solid-phase extraction method consumes It takes a long time, and it usually takes 3-4 hours to complete the detection of a water sample

Method used

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  • Method for determining antibiotics in water by solid-phase extraction-liquid chromatography-tandem mass spectrometry by using special column for large-volume water sample
  • Method for determining antibiotics in water by solid-phase extraction-liquid chromatography-tandem mass spectrometry by using special column for large-volume water sample

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Experimental program
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Effect test

Embodiment 1

[0034] S10, activating the Cleanert LDC solid-phase extraction column with 5mL methanol and 5mL0.1% formic acid;

[0035] S20, take 1L tap water sample, add 0.25gNa 2 EDTA and 1mol / L dilute hydrochloric acid solution, adjust the pH to 4.0, and set aside;

[0036] S30. Rapidly pass the water sample prepared in step 2 through the Cleanert LDC solid-phase extraction column at a flow rate of 90 mL / min, and the extraction time is 15 minutes to enrich the residual antibiotics in the water;

[0037] S40, eluting the residual antibiotics in the water body enriched in step 3 with 20 mL of 5% ammonia water and methanol, blowing with nitrogen and concentrating to near dryness; dissolving and constant volume with 1.0 mL of 10% acetonitrile to obtain the solution to be tested;

[0038] S50. Filter the liquid to be tested in step 4 through a 0.22 μm organic filter membrane, and then put it into an LC-MS / MS detection device for liquid chromatography tandem mass spectrometry detection to obt...

Embodiment 2

[0040] S10, activating the Cleanert LDC solid-phase extraction column with 5mL methanol and 5mL0.1% formic acid;

[0041] S20, take 1L Minjiang water sample, add 0.25gNa 2 EDTA and 1mol / L dilute hydrochloric acid solution, adjust the pH to 4.0, and set aside;

[0042] S30. Rapidly pass the water sample prepared in step 2 through the Cleanert LDC solid-phase extraction column at a flow rate of 90 mL / min, and the extraction time is 15 minutes to enrich the residual antibiotics in the water;

[0043] S40, eluting the residual antibiotics in the water body enriched in step 3 with 20 mL of 5% ammonia water and methanol, blowing with nitrogen and concentrating to near dryness; dissolving and constant volume with 1.0 mL of 10% acetonitrile to obtain the solution to be tested;

[0044] S50. Filter the liquid to be tested in step 4 through a 0.22 μm organic filter membrane, and then put it into an LC-MS / MS detection device for liquid chromatography tandem mass spectrometry detection t...

Embodiment 3

[0046] S10, activating the Cleanert LDC solid-phase extraction column with 5mL methanol and 5mL0.1% formic acid;

[0047] S20, take 1L Fuzhou inland river water sample, add 0.25gNa 2 EDTA and 1mol / L dilute hydrochloric acid solution, adjust the pH to 4.0, set aside;

[0048] S30. Rapidly pass the water sample prepared in step 2 through the Cleanert LDC solid-phase extraction column at a flow rate of 90 mL / min, and the extraction time is 15 minutes to enrich the residual antibiotics in the water;

[0049] S40, the residual antibiotics in the water body enriched in step 3 were eluted with 20mL of 5% ammonia water methanol, concentrated to near dryness by nitrogen blowing; dissolved in 1.0mL of 10% acetonitrile to obtain the test solution;

[0050] S50. Filter the liquid to be tested in step 4 through a 0.22 μm organic filter membrane, and then put it into an LC-MS / MS detection device for liquid chromatography tandem mass spectrometry detection to obtain the contents of 40 kinds...

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Abstract

The invention provides a method for determining antibiotics in water by solid-phase extraction-liquid chromatography-tandem mass spectrometry by using a special column for a large-volume water sample.The method comprises the steps of (1) activating a special column for large-volume water by using methanol and formic acid; (2) taking an appropriate amount of water sample to quickly pass through the special column for the large-volume water at a certain flow velocity and enriching residual antibiotics in a water body; (3) eluting the residual antibiotics, enriched in the step (2), in the waterbody by using ammonia methanol, carrying out nitrogen blowing concentration until the residual antibiotics are nearly dry, dissolving the residual antibiotics by using acetonitrile until constant volume and obtaining a test solution; and (4) filtering the test solution obtained in the step (3) through an organic filter membrane, carrying out liquid chromatography-tandem mass spectrometry detectionand collecting and processing measured data of the antibiotics in the water body. According to the method, fast sample loading is carried out by adopting the special column for the large-volume water, the sample loading time of 1L of water sample can be compressed to 11-15min and the whole preprocessing time can be compressed to half an hour, so that a fast and reliable experimental method is provided for detection of five types of 40 antibiotics in the water body.

Description

technical field [0001] The invention relates to the technical field of antibiotic detection in water, in particular to a method for determining antibiotics in water with a special column for large-volume water samples, solid-phase extraction-liquid chromatography tandem mass spectrometry. Background technique [0002] Antibiotics are important components in pharmaceuticals and personal care products, and are widely used in animal farming. However, most antibiotics cannot be completely absorbed, and some antibiotics enter the water environment in different forms. For example, sulfamethoxazole is often detected in domestic wastewater, surface water, and even drinking water. With the improvement of living standards, the standards of people's livelihood needs in all aspects have also been continuously improved. Therefore, the problem of water pollution by antibiotics is gradually attracting people's attention. It is known that antibiotics have a cumulative effect after remain...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/36G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/36G01N30/7266G01N30/8679G01N2030/027
Inventor 李文最吴良康李伟弘
Owner 福建浩得实验室系统科技有限公司
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