Method for separating and enriching sulfonamide antibiotics in drinking water

A technology for separation and enrichment of sulfonamides, applied in material separation, analysis of materials, measuring devices, etc., can solve problems such as inability to completely remove sulfonamides, poor adhesion of sulfonamides, and impact on groundwater quality and safety, and achieve sample detection High efficiency, short enrichment time, and highly reproducible results

Inactive Publication Date: 2019-10-25
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, sulfa drugs have poor adhesion and strong mobility in the soil, and the polluted surface water will affect the water quality of the local and surrounding groundwater. The current purification process of the waterworks cannot completely remove the sulfa drugs in the water. The method of collecting sulfonamides in groundwater and drinking water is the premise of accurate and quantitative detection of their residual levels, which has important practical significance for the analysis of water environmental pollution and the assessment of human health risks

Method used

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  • Method for separating and enriching sulfonamide antibiotics in drinking water
  • Method for separating and enriching sulfonamide antibiotics in drinking water
  • Method for separating and enriching sulfonamide antibiotics in drinking water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Take 1000 mL of ultrapure water in a brown glass bottle, add 0.1 mL of 9 kinds of sulfonamide antibiotic mixed standard working solution with a concentration of 500 μg / L to each bottle of water sample, adjust the pH of the water sample to 3 with acid, and use GF / F (Whatman, 0.45 μm) glass fiber membrane filtration. The pretreated water samples were obtained.

[0026] (2) Use 10 mL methanol and 10 mL ultrapure water in sequence to activate the MCX (Shanghai Anpu Company, 500 mg, 6 cc) solid-phase extraction column, so that the resin in the solid-phase extraction column is in an activated state. Take 1000 mL of the step ( 1) The obtained pretreated water sample was passed through the column, and the filtration flow rate was controlled at 4 mL / min; after the enrichment was completed, the extraction column was dried with nitrogen for 30 min, and the solid was rinsed with 10 mL of ultrapure water with a pH value of 3. Phase extraction column, to remove the water-soluble...

Embodiment 2

[0043] Take 1000 mL of tap water sample in a brown bottle, and add the standard to the water sample according to the method in Example 1. At the same time, take 1000 mL of the water sample without adding the standard, as a blank control.

[0044] The results of the spiked water samples were brought into the standard curve equation, and the concentrations of the nine sulfonamide antibiotics in the water samples to be tested were finally obtained by calculation. The recovery rate was calculated, and the results are shown in Table 3.

Embodiment 3

[0046] 1000 mL of groundwater samples from villages near Guilin Huixian Wetland were collected in brown glass bottles, 0.1 mol / L hydrochloric acid was added to adjust the pH of the water samples to 3, and they were stored below 4°C and transported back to the laboratory. The water sample was pretreated according to the method in Example 1, and then detected by high-performance liquid chromatography-ultraviolet detector (HPLC-UVD), and brought into the standard curve equation to finally obtain the 9 sulfonamides in the actual water sample by calculation The concentration of antibiotics. Calculate the recovery rate, and the results are shown in Table 4.

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Abstract

The invention discloses a method for separating and enriching sulfa antibiotics in drinking water. The method comprises a step of adjusting the pH of a water sample to 3 to 4 with acid and filtering to obtain a preprocessed water sample, a step of sequentially activating an MCX solid phase extraction column with methanol and ultrapure water and allowing sampled water to pass through the column, astep of drying the MCX solid phase extraction column under the protection of nitrogen after the enrichment is completed, rinsing the column with ultrapure water with pH of 3 to remove water-soluble interference impurities of the water sample enriched on the MCX solid phase extraction column, eluting with a methanol solution containing 8-15% ammonia water, slowly blowing an eluate with nitrogen stream to be nearly dry, and adding an aqueous solution re-dissolved residue containing methanol to complete the separation and enrichment of the sulfa antibiotics in the drinking water. The method of the invention has the advantages of simple operation, environmental friendliness and high enrichment ratio, multiple drugs of the same type of antibiotics and other drugs with similar physical and chemical properties to sulfonamides can be simultaneously enriched, the method is particularly suitable for the separation detection of trace sulfonamide antibiotics in a drinking water body, and the accuracy is high.

Description

technical field [0001] The invention belongs to the technical field of detection pretreatment of trace organic pollutants in drinking water and groundwater, and particularly relates to a method for separating and enriching sulfonamide antibiotics in drinking water. Background technique [0002] Sulfonamides (SAs) are the earliest antibacterial drugs that were synthesized and successfully applied to human bacterial infectious diseases. Because of its broad antibacterial spectrum and low price, it is widely used in aquaculture, animal husbandry and clinical medical treatment. [0003] With the rapid development of the breeding industry, sulfa drugs are widely used in animal breeding, and have become the second largest veterinary drug antibiotics. According to the data of FDA (US Food and Drug Administration), there are about 43 antibiotics in the United States. % of livestock antibiotics are used in cattle breeding, where sulfonamides are difficult to be absorbed and metaboli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08
CPCG01N30/02G01N30/06G01N30/08G01N2030/062
Inventor 曾鸿鹄梁延鹏庞昕瑞覃礼堂莫凌云
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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