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A simultaneous extraction method of multiple residual drugs in environmental water

An environment and water body technology, applied in the direction of instruments, measuring devices, scientific instruments, etc., can solve the problem that multiple drug residues cannot be extracted at the same time, achieve rapid quantitative detection with high selectivity and high sensitivity, optimize extraction conditions, and meet the detection requirements effect of demand

Active Publication Date: 2021-07-20
JINAN UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the technical defects and deficiencies in the prior art that multiple drug residues in the water cannot be extracted simultaneously, and provide a fast and efficient simultaneous extraction method for multiple antibiotics and endocrine disruptor drugs in the water environment

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  • A simultaneous extraction method of multiple residual drugs in environmental water

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Effect test

Embodiment 1

[0056] Example 1 Optimization of solid-phase extraction elution conditions

[0057] Select 9 antibiotics commonly found in the environment (sulfapyridine, sulfadiazine, sulfamethazine, sulfamethoxazole, roxithromycin, tetracycline, ofloxacin, norfloxacin, ciprofloxacin) and 5 kinds of endocrine disruptors (estrone, nonylphenol, bisphenol A, triclocarban, triclosan) residual drugs, using a single factor impact test to investigate the enriched antibiotics and endocrine disruptors in the HLB solid-phase extraction column According to the different elution conditions of prime drugs, the optimal elution conditions were selected based on the best recovery rate and standard deviation data.

[0058] The results showed that the optimal SPE elution collection process was as follows:

[0059] The elution method is to use 5mL 10% methanol-acetic acid solution for the first elution, the eluate is collected and transferred to a glass tube, and then 10mL 5% methanol-2% acetic acid acid wash...

Embodiment 2

[0061] Example 2 Simultaneous extraction and quantitative detection test of multiple antibiotics and environmental hormones in sewage

[0062] Utilizing the optimized solid-phase extraction elution conditions in Example 1, combined with ultra-high performance liquid chromatography-mass spectrometry, nine kinds of antibiotics and five kinds of endocrine disruptor drugs in environmental water samples were quantitatively detected. At the same time, the conditions of chromatography and mass spectrometry were optimized.

[0063] A simultaneous extraction and quantitative detection method of multiple antibiotics and environmental hormones in sewage, the specific steps are as follows:

[0064] (1) Pretreatment of sewage samples

[0065] Collect 1000 mL sewage samples, after Whaterman's Φ = After filtering through a 0.7 μm glass fiber membrane, add 0.6 g of EDTA sodium salt chelating agent, and at the same time add 50 mL of chromatographic grade methanol, and mix well.

[0066] (2...

Embodiment 3

[0077] Example 3 Extraction and quantitative detection test of 14 kinds of antibiotics and environmental hormones in campus sewage

[0078] 1. Experimental method

[0079] Collect 1000 mL of campus domestic sewage, and process and test the campus domestic sewage samples according to the method in Example 2.

[0080] 3. Experimental results

[0081] (1) The linear relationship and sensitivity of the detection method

[0082] Under the above chromatographic and mass spectrometry conditions, sulfapyridine, sulfadiazine, sulfamethazine, sulfamethoxazole, roxithromycin, tetracycline, ofloxacin, norfloxacin, ciprofloxacin, estrogen The correlation coefficients of the standard curves for ketone, nonylphenol, bisphenol A, triclocarban, and triclosan were as high as 0.9984, the detection limit of the instrument was 0.005-0.326 µg / L, and the limit of quantification was 0.018-0.416 µg / L.

[0083] (2) Extraction recovery rate

[0084] 100 μg / L of each substance to be tested was added ...

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Abstract

The invention discloses a method for simultaneously extracting multiple residual medicines in environmental water bodies. For the first time, the method adopts the acid-base eluent graded elution of methanol and the graded eluting method of methanol-containing acid wash solution and alkali wash solution, which simplifies and optimizes the pretreatment and extraction conditions of antibiotics and endogenous interferon drugs in water samples. , eliminating the silica gel column purification step after the traditional solid-phase extraction method for endocrine disruptor drugs, improving the selectivity and enhancing the peak response intensity of the analyte. At the same time, the extraction method of the present invention combined with ultra-high performance liquid chromatography-mass spectrometry technology can achieve high selectivity, high sensitivity, rapid and simultaneous quantitative detection of various antibiotics and endocrine disruptor drugs in the water environment, which can meet the requirements of various environmental water bodies. It has a good application prospect for the detection needs of middle and trace drugs.

Description

technical field [0001] The invention belongs to the technical field of environmental detection. More specifically, it relates to a method for simultaneous pretreatment and extraction of multiple antibiotics and endocrine disruptor drugs in environmental water. Background technique [0002] The detection of drug residues in environmental water is of great significance for the monitoring of environmental water and the assessment and prevention of drug pollution. Antibiotics and endocrine disruptors are common drug residues in water. There are many kinds of antibiotics, and they are widely used in a wide range of applications. Because of their functions of preventing and treating diseases and promoting growth, they are widely used in human and animal medicine and livestock breeding. After antibiotics enter the human body or animals, only a small part is absorbed, and about 10% to 90% are discharged into the environment in the form of original drugs along with animal feces. A...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/08
Inventor 邰义萍阮伟峰杨扬王瑞陶然蔡红波
Owner JINAN UNIVERSITY
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