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Method for simultaneously detecting tetracycline antibiotics in water

A detection method and a tetracycline-based technology, which are applied to measurement devices, instruments, scientific instruments, etc., can solve the problems of difficulty in measuring sensitivity, cumbersome operation, poor specificity, etc. of photometric method and TLC method, and achieve simple and easy operation and analysis. Fast, easy-to-operate effects

Inactive Publication Date: 2013-10-02
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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Problems solved by technology

[0003] There are many detection methods for the residues of tetracycline antibiotics, such as microbial method, ELISA, UV spectrophotometry, fluorescence photometry and thin layer chromatography (TLC), etc., wherein the microbiological method and ELISA have poor specificity and consume a lot of time. However, the measurement sensitivity of the photometric method and TLC method is difficult to meet the requirements

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  • Method for simultaneously detecting tetracycline antibiotics in water
  • Method for simultaneously detecting tetracycline antibiotics in water
  • Method for simultaneously detecting tetracycline antibiotics in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Embodiment 1: recovery rate experimental result

[0053] (1) Take 1000ml of ultrapure water in a brown glass bottle, add 1ml of 100μg / L three tetracycline antibiotics mixed standard stock solution to each bottle of water sample, mix well, add a small amount of hydrochloric acid to adjust the pH of the water sample to about 3.0.

[0054] (2) Concentration and enrichment

[0055]Utilize 6mL chromatographically pure acetone, 6mL chromatographically pure methanol, 6mL 0.1% (m / v) formic acid aqueous solution containing 5mmol / L ammonium acetate, and 15-20mL ultrapure water to activate the HLB (500mg, 6cc) solid phase extraction column of Waters Company successively , control the flow rate to be less than 1mL / min; after the enrichment is completed, dry the small column under nitrogen protection for 20min, use 10mL chromatographically pure methanol solution to elute the HLB column, control the flow rate to be less than 1mL / min, and collect the eluate in 10mL conical bottom glas...

Embodiment 2

[0060] Example 2: Recovery results of water samples from Beijing Olympic Park

[0061] Take 1000ml of river water samples from Beijing Olympic Park in a brown glass bottle, and carry out the standard addition experiment according to the method in Example 1, while taking 1000ml of river water samples without adding standards, as a blank control.

[0062] The results of the water samples after adding the standard were brought into the standard curve equation, and the concentrations of the three tetracycline 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 2.

Embodiment 3

[0063] Example 3: Measurement results of actual water samples in Wangyanggou, Shijiazhuang, Hebei.

[0064] 1000mL water samples from Ziyahe Wangyanggou (37°35′36″N; 114°25′15″E) were subjected to negative pressure suction filtration through a glass fiber membrane (Whatman, 0.45μm), and the filtrate was subjected to 6mL chromatographic analysis beforehand. Pure acetone, 6mL chromatographically pure methanol, 6mL 0.1% (m / v) formic acid aqueous solution containing 5mmol / L ammonium acetate, 15-20mL ultrapure water activate the HLB cartridge, and control the flow rate at 2-5mL / min. Vacuum dry for 1 min after the enrichment, 10mL pure methanol solution to elute the HLB column, collect the eluate in a 10mL pointed-bottom glass colorimetric tube, blow the eluate slowly under nitrogen flow until nearly dry, add 400μL chromatographically pure acetonitrile to dissolve The residue, vortexed, was assayed.

[0065] The concentrations of the three tetracycline antibiotics in the above samp...

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Abstract

The invention discloses a method for detecting trace tetracycline antibiotics in water. The method comprises the following steps of: filtering a water sample to remove suspensions, and adjusting the pH of the water sample to 2-4; activating a hydrophile lipophile balance (HLB) solid-phase extraction column sequentially by using acetone, methyl alcohol, a methanoic acid aqueous solution containing ammonium acetate and super-pure water, taking a water sample through column in the step (1), drying the HLB solid-phase extraction column under nitrogen protection, eluting the HLB solid-phase extraction column by eluant, collecting the eluant, drying the eluant under nitrogen flow, and adding acetonitrile to dissolve residues; and quantitatively detecting the concentration of the trace tetracycline antibiotics. The method is environmentally-friendly in water sample pretreatment environment, easy to operate, high in enrichment coefficient and high in reproducibility and has the advantages of quickness, accuracy, high sensitivity, wide application range and the like.

Description

technical field [0001] The invention belongs to the technical field of detection of water environmental pollutants, in particular to a detection method for simultaneously detecting trace amounts of tetracycline antibiotics in water bodies, more specifically for trace amounts of tetracycline, oxytetracycline, and gold in surface water (river water). Method for the detection of mycotoxin. Background technique [0002] Tetracycline antibiotics include oxytetracycline (OTC), tetracycline (TC) and chlortetracycline (CTC), etc., which are broad-spectrum antibiotics. Because of their good bactericidal or bacteriostatic effects, they are widely used in the prevention and treatment of animals and aquatic products. disease infection. Tetracycline antibiotics can promote the growth of livestock and poultry when used in low doses, and can treat diseases when used in high doses, so they have been widely used in livestock and poultry breeding. Tetracycline antibiotics, as broad-spectrum...

Claims

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Application Information

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IPC IPC(8): G01N30/08G01N30/02
Inventor 席北斗薛成丁京涛高如泰许其功曹金玲张媛
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI
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