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Pretreatment method and detection method of amoxicillin, penicillin G and penicillin V

A detection method and pretreatment technology, which are applied in the field of pretreatment, can solve the problems of long time consumption, large amount of organic solvent used, and many operation steps of the solid phase extraction pretreatment method.

Active Publication Date: 2016-06-01
BRIGHT DAIRY & FOOD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the problem of the solid phase of the prior art before detecting the content of one or more of amoxicillin, penicillin G and penicillin V remaining in raw milk and / or liquid milk products. The extraction pretreatment method has the defects of many operation steps, long time consumption and large amount of organic solvents, and provides a pretreatment method and a detection method for amoxicillin, penicillin G and penicillin V

Method used

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  • Pretreatment method and detection method of amoxicillin, penicillin G and penicillin V

Examples

Experimental program
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Effect test

Embodiment 1

[0067] Preparation of standard curve:

[0068] Weigh 10 mg (accurate to 0.1 mg) of each standard substance of amoxicillin, penicillin G and penicillin V, prepare a single standard stock solution with a concentration of 1000.0 mg / Kg with acetonitrile, and store all solutions at 4°C in the dark. Pipette an appropriate amount of standard solution before use, and gradually dilute the blank sample extract to form a mixed standard working solution. In the mixed standard working solution, the concentrations of amoxicillin, penicillin G, and penicillin V are 4 μg / Kg, 5 μg / Kg, 10 μg / Kg, 30 μg / Kg, 20 μg / Kg, 40 μg / Kg, 100 μg / Kg, 140 μg / Kg and 200 μg / Kg. Sample injection was performed by high-performance liquid chromatography-electrospray spray tandem secondary mass spectrometry (LC-MS / MS) detection, and a standard curve was prepared.

[0069] The conditions for high performance liquid chromatography detection are:

[0070] Column: WaterxselectC 18 column(4.6mm×250mm);

[0071] Column...

Embodiment 2

[0097] 1. Pretreatment of samples to be tested

[0098] (1) Weigh 1 g (accurate to 0.01 g) of raw milk (this is a blank sample without the three components to be tested) as sample A and sample B, and place them in 10 mL polypropylene centrifuge tubes. Add the 20 μg / Kg mixed standard solution (final concentration after constant volume) of Example 1 to sample A, mix well, and use it as sample A to be tested. Sample B is left without any treatment and is used as sample B to be tested. Both sample A and sample B to be tested are processed as follows: add 0.2% formic acid and 4 mL of acetonitrile, vortex for 3 minutes, centrifuge at a speed of 5000 rpm for 5 minutes, pipette the supernatant into a 10 mL volumetric flask; Add 0.2% formic acid and 4 mL of acetonitrile, repeat the above extraction steps, combine the two extracts, and adjust the volume of acetonitrile to 10 mL; the above percentages are the volume percentages of formic acid in the amount of acetonitrile added;

[009...

Embodiment 3

[0113] 1. Pretreatment of samples to be tested:

[0114] (1) Weigh 1 g (accurate to 0.01 g) of raw milk (this is a blank sample without the three components to be tested) as sample A and sample B, and place them in 10 mL polypropylene centrifuge tubes. Add the 50 μg / Kg mixed standard solution (final concentration after constant volume) of Example 1 to sample A, mix well, and use it as sample A to be tested. Sample B is left without any treatment and is used as sample B to be tested. Both sample A and sample B to be tested were processed as follows: add 0.1% formic acid and 10mL acetonitrile, vortex for 1min, centrifuge at 5000rpm for 5min, pipette the supernatant into a 25mL volumetric flask, and pour into the sample to be tested Add 0.1% formic acid and 10 mL of acetonitrile to the mixture, repeat the above extraction steps, combine the two extracts, and dilute the water to 25 mL; the above percentages are the volume percentages of formic acid in the amount of acetonitrile a...

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Abstract

The invention discloses a pretreatment method and a detection method of amoxicillin, penicillin G and penicillin V. The pretreatment method comprises the following steps that 1, a mixture of a sample to be detected and acetonitrile is centrifuged to collect supernatant, and the sample to be detected is a milk product which does not contain solid particles; 2, the supernatant is loaded to an activated Oasis PRiME HLB solid-phase extraction column, and effluent is collected. The pretreatment method is fast, simple, economical, reliable, capable of effectively extracting components to be detected and removing the influence of a complex matrix, and beneficial for fast detecting the sample to be detected. While the high extraction rate is kept, less organic solvent is used and discharged, loss of the organic solvent is reduced, environment is protected easily, the pretreatment steps are reduced, time is saved, energy consumption is reduced, and the detection method is fast, simple and high in precision and accuracy, and has high application value.

Description

technical field [0001] The invention relates to a pretreatment method and a detection method for amoxicillin, penicillin G and penicillin V. Background technique [0002] Amoxicillin, penicillin G and penicillin V are the most commonly used veterinary drugs in animal husbandry. They all belong to the β-lactam antibiotics and are broad-spectrum penicillin antibiotics. Amoxicillin, also known as amoxycillin or amoxycillin, has strong bactericidal effect and strong ability to penetrate cell membranes, and is one of the most widely used oral penicillins at present. Penicillin G is also known as penicillin, penicillin sodium, benzyl penicillin sodium, penicillin potassium or benzyl penicillin potassium. Penicillin G is a kind of antibiotic. It is a class of antibiotics that contain penicillane in the molecule extracted from the culture solution of Penicillium, can destroy the cell wall of bacteria and play a bactericidal effect during the reproduction period of bacterial cells. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/062
Inventor 王渊龙游春苹刘振民
Owner BRIGHT DAIRY & FOOD
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