Method for separation and enrichment of penicillin antibiotics in water

A technology for separation, enrichment and neutralization of penicillin. It is used in material separation, material analysis, and measurement devices. It can solve the problems of easy hydrolysis and instability of penicillin antibiotics, and achieve high sample detection efficiency, strong repeatability, and high stability. Accurate effect

Inactive Publication Date: 2013-10-09
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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Problems solved by technology

The results of the study showed that the content of penicillin antibiotics in environmental water samples was very sma

Method used

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  • Method for separation and enrichment of penicillin antibiotics in water
  • Method for separation and enrichment of penicillin antibiotics in water
  • Method for separation and enrichment of penicillin antibiotics in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment 1: recovery rate experimental result

[0049] Take 1000ml of ultrapure water in a brown glass bottle, add 1ml of 100μg / L mixed standard stock solution of two kinds of penicillin antibiotics to each bottle of water sample, mix well, process the water sample according to step 1-2, and finally use high performance liquid chromatography-tandem mass spectrometry Combined determination of the concentration of two penicillin antibiotics. figure 1 It is the ion chromatogram of the mixed standard solution of two penicillin antibiotics at 100 μg / L, and the peak order is sulbactam: 1.85min; cloxacillin: 4.81min.

[0050] Drawing of standard curve by external standard method: dilute the stock solution with pure acetonitrile to two penicillins with serial concentrations of 10μg / L, 20μg / L, 50μg / L, 100μg / L, 200μg / L, 500μg / L and 1000μg / L Antibiotics were mixed with standard solutions, transferred to sampling vials, and determined by high performance liquid chromatography-ta...

Embodiment 2

[0052] Example 2 The recovery results of water samples from Beijing Olympic Park.

[0053] 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.

[0054] The results of the water samples after adding the standard were brought into the standard curve equation, and the concentrations of the three penicillin 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

[0055] Example 3 Determination results of water samples in Wangyanggou, Shijiazhuang, Hebei.

[0056] Use a brown glass bottle to collect 1000ml of water samples from Wangyanggou, Shijiazhuang, Hebei, add about 3mL of 4M hydrochloric acid to adjust the pH to about 3.0, store it below 4°C and transport it back to the laboratory. Filter with GF / F (Whatman, 0.7 μm) glass fiber filter membrane, concentrate and enrich the water sample according to steps (2) to (3), and then perform liquid chromatography-tandem mass spectrometry detection according to step (4), and bring Into the standard curve equation, the concentration of the two penicillin antibiotics in the actual water sample was finally obtained by calculation. The test results in Table 3 show that there are almost no residues of sulbactam and cloxacillin in Wangyanggou.

[0057] Table 1

[0058]

[0059] Table 2

[0060]

[0061] table 3

[0062]

[0063] Nd = not detect.

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Abstract

The invention relates to a method for separation and enrichment of penicillin antibiotics in water. The method comprises the following steps of adjusting a pH value of a water sample to 2-4 by an acid; filtering the water sample to obtain a pretreated water sample; activating an HLB solid-phase extraction column by acetone, methanol and a formic acid aqueous solution containing ammonium acetate successively; adding ultrapure water to keep a resin in the HLB solid phase extraction column in an activated state; passing the water sample through the column; drying the HLB solid-phase extraction column under the protection of nitrogen after enrichment is finished; eluting with an eluent; collecting the eluent; blow-drying under a nitrogen flow; adding acetonitrile to dissolve residual materials for detection; and detecting the concentrations of penicillin antibiotics quantitatively. The method is advantageous in that the pretreatment of the water sample is environment-friendly; and the method can be operated easily, has high enrichment coefficient, low detection limit and good repeatability, and can analyze the content of two trace penicillin antibiotics in a water environment rapidly and accurately.

Description

technical field [0001] The present invention relates to a detection pretreatment method of trace penicillin antibiotics in water environment, specifically a method for simultaneously separating and enriching two trace penicillin antibiotics-sulbactam and chlorazole in surface water and urban sewage Xilin's method. Background technique [0002] Penicillin antibiotics refer to a class of antibiotics that contain penicillane in the molecule, which can destroy the cell wall of bacteria and play a bactericidal effect during the reproduction period of bacterial cells. It has a strong selective effect on bacteria and has almost no toxicity to humans. Therefore, it is an important antibiotic with high efficiency, low toxicity and is widely used in clinical practice. [0003] Penicillin antibiotics rank among the best in the amount of antibiotics used in my country due to their strong bactericidal effect, excellent curative effect, low toxicity, and low price. The abuse of penicill...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08
Inventor 高如泰邵一如张媛张慧许其功曹金玲
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI
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