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Detection method for simultaneously measuring residue of tetracyclines (TCs) drugs in royal jelly

A technology of tetracycline drugs and detection methods, applied in the direction of measuring devices, instruments, scientific instruments, etc.

Inactive Publication Date: 2009-11-04
THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the difficult problem of detection of multiple tetracycline drug residues in the existing royal jelly, the H of the present invention is to provide a simultaneous and convenient detection method for multiple tetracycline drug residues in royal jelly using liquid chromatography-mass spectrometry / mass spectrometry

Method used

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  • Detection method for simultaneously measuring residue of tetracyclines (TCs) drugs in royal jelly
  • Detection method for simultaneously measuring residue of tetracyclines (TCs) drugs in royal jelly
  • Detection method for simultaneously measuring residue of tetracyclines (TCs) drugs in royal jelly

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Experimental program
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Embodiment Construction

[0027] 1. Sample processing method

[0028] 1. Extraction

[0029] Weigh 2g of royal jelly (accurate to 0.01g) and place it in a 50mL centrifuge tube, add 5mL LEDTA-McIlvaine buffer solution (EDTA-McIlvaine buffer solution: weigh 60.5g disodium ethylenediaminetetraacetic acid, add 1625mL McIlvaine buffer solution (625mL Mix 0.2mol / L disodium hydrogen phosphate solution with 1000mL 0.1mol / L citric acid solution, adjust pH=4.0 with phosphoric acid, dissolve it and shake well), mix well, then add 5ml methanol and mix well, centrifuge at 4000r / min 10min, the supernatant was transferred to a 50mL volumetric flask. Add 10mL EDTA-McIlvaine buffer solution to the lower sediment, mix well, centrifuge at 4000r / min for 10min, and then transfer the supernatant to a 50mL volumetric flask. Repeat the operation once. Dilute the extract to 50 mL with EDTA-McIlvaine buffer solution. Use 1mol / L sodium hydroxide solution to adjust the pH to 6.0 for purification.

[0030] 2. Purification

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Abstract

The invention relates to a detection method for simultaneously measuring the residue of tetracyclines (TCs) drugs in royal jelly, in particular to a detection method for simultaneously measuring the residue of 10 veterinary drugs including oxytetracycline, tetracycline, demethylchlortetracycline, chlorotetracycline, doxycycline, 4- epioxytetracycline, 4-epitetracycline, 4-epichlorotetracycline, minocycline and methacycline. The method comprises the following steps: precipitating protein by methanol; then, adjusting the pH value; further carrying out multi-stage purification; and simply and simultaneously measuring the residue of the TCs drugs by the liquid chromatography-mass spectrometry / mass spectrometer (LC-MS / MS). By carrying out the pre-treatment for one time, the invention can measure the residue of up to 10 TCs drugs in the royal jelly, wherein, the lower limits of detection (LLD) of the five TC antibiotics including oxytetracycline, tetracycline, demethylchlortetracycline, chlorotetracycline and doxycycline are 2.0 mug / kg; while the LLDs of the other veterinary drugs including 4- epioxytetracycline, 4-epitetracycline, 4-epichlorotetracycline, minocycline and methacycline are 10.0 mug / kg.

Description

technical field [0001] The present invention relates to the method for the detection of tetracycline drug residues in royal jelly, especially relate to oxytetracycline, tetracycline, demeclotetracycline, chlortetracycline, doxycycline, 4-epi-oxytetracycline, 4-epi-tetracycline, 4- Poor to the detection of 10 kinds of veterinary drugs such as aureomycin, minocycline and methacycline. Background technique [0002] Tetracyclines (Tetracyclines, TCs) are a class of broad-spectrum antibiotics produced by Streptomyces, and they all belong to the derivatives of polycyclic tetracenecarboxamide core in chemical structure. In livestock and poultry production, tetracyclines are widely used as drug additives to prevent intestinal infection, promote growth and increase milk production of dairy cows. It is also widely used in aquaculture and beekeeping to prevent and treat various infectious diseases. [0003] However, because tetracyclines are mainly excreted by glomerular filtration i...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/06
Inventor 黄超群陈笑梅谢文丰金平刘海山丁慧瑛
Owner THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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