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Method for detecting residual quantity of norfloxacin antibiotic in milk

A norfloxacin and detection method technology is applied in the field of detection of norfloxacin antibiotic residues in milk, which can solve the problems of long detection time and high detection limit of norfloxacin antibiotics, and achieve short detection time and reduce The probability of false positive (negative) test results and the effect of strong selectivity

Inactive Publication Date: 2009-12-23
INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, with this method, the detection time is longer, and the detection limit of norfloxacin antibiotics detected by high performance liquid chromatography is relatively high (generally higher than 20 μg / kg).

Method used

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  • Method for detecting residual quantity of norfloxacin antibiotic in milk
  • Method for detecting residual quantity of norfloxacin antibiotic in milk
  • Method for detecting residual quantity of norfloxacin antibiotic in milk

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1 The content of the norfloxacin antibiotic norfloxacin in milk was determined by ultra-high performance liquid chromatography-electrospray tandem triple quadrupole mass spectrometer (WatersTQD).

[0036] 1) Preparation of standard solution:

[0037] Precisely weigh 10 mg of norfloxacin standard substance, dilute it in a 100 mL brown volumetric flask with methanol, and mix well to obtain a standard stock solution with a concentration of norfloxacin of 100 μg / mL, and store it in a -18°C freezer away from light , for at least 4 weeks. When in use, dilute to 100ng / mL, 50ng / mL, 20ng / mL, 10ng / mL, 5ng / mL standard solutions.

[0038] 2) Preparation of reagents:

[0039] (a) Preparation of extract:

[0040]0.2mol / L disodium hydrogen phosphate solution: Accurately weigh 28.41g of disodium hydrogen phosphate, dissolve in water, and dilute to 1000mL.

[0041] 0.1mol / L citric acid solution: Accurately weigh 21.01g of citric acid, dissolve in water, and dilute to 1000mL....

Embodiment 2

[0068] Example 2 The content of norfloxacin in milk was determined by ultra-high performance liquid chromatography-electrospray tandem triple quadrupole mass spectrometer (WatersTQD).

[0069] 1) Preparation of standard solution: same as the preparation of standard solution in Example 1.

[0070] 2) Preparation of reagents:

[0071] (a) Preparation of extract: same as Example 1.

[0072] (b) preparation of mobile phase: with embodiment 1.

[0073] 3) Sample preparation:

[0074] Weigh 5.0000g milk sample, put it in a 50mL polypropylene centrifuge tube, add 20mLNa 2 The EDTA-Mellvaine buffer solution was fully shaken at room temperature for 2 minutes, allowed to stand for 15 minutes, fully extracted, then added 1 mL of 50% trichloroacetic acid to mix, and centrifuged at 10,000 rpm at 4°C for 10 minutes to obtain a supernatant to be purified.

[0075] Use 5.0mL methanol to pass through the solid-phase extraction column at a flow rate of 1.0-2.0mL / min, and then use 10.0mL ult...

Embodiment 3

[0087] Example 3 The content of norfloxacin in milk was determined by ultra-high performance liquid chromatography-electrospray tandem triple quadrupole mass spectrometer (WatersTQD).

[0088] 1) Preparation of standard solution: same as Example 1.

[0089] 2) Preparation of reagents:

[0090] (a) preparation of extract: with embodiment 1

[0091] (b) preparation of mobile phase: with embodiment 1

[0092] 3) Sample preparation:

[0093]Weigh 3.0000g milk sample, put it in a 50mL polypropylene centrifuge tube, add 30mLNa 2 The EDTA-Mellvaine buffer solution was fully shaken at room temperature for 2 minutes, allowed to stand for 15 minutes, fully extracted, then added 5 mL of 50% trichloroacetic acid to mix, and centrifuged at 10,000 rpm and 4°C for 10 minutes to obtain a supernatant to be purified.

[0094] Use 5.0mL methanol to pass through the solid-phase extraction column at a flow rate of 1.0-2.0mL / min, and then use 10.0mL ultrapure water to pass through the column at...

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Abstract

The invention relates to a method for detecting residual quantity of norfloxacin antibiotic in milk. The method utilizes an ultra-performance liquid chromatography (UPLC)-electrospray tandem triple quadrupole mass spectrometer to determine the residual quantity of norfloxacin antibiotic. A sample is extracted by Na2 EDTA-Mellvaine buffer solution (pH 4.0), subjected to protein removal by trichloroacetic acid, purified and concentrated by a PEP solid phase extraction columella, separated by adopting a chromatographic column with column temperature of 30 DEG C, subjected to gradient elution by adopting aqueous solution (v / v) containing 0.1% formic acid and acetonitrile as a flowing phase, and then quantitated by adopting a multiple reaction monitoring manner. The instrument detection limit is 1.0-2.0 mug / Kg; and within the linear range of 1-100 mug / Kg, the correlation coefficient r can reach more than 0.999, and the coefficient of recovery is 80%-105% (adding level of 10, 50 and 100 mug / Kg). The method has the advantages of rapidness, accuracy, high sensitivity and wide application scope.

Description

technical field [0001] The invention relates to a method for detecting antibiotic content in milk, in particular to a method for detecting antibiotic residue of norfloxacin in milk. It belongs to the field of analysis technology. Background technique [0002] Norfloxacin is a broad-spectrum high-efficiency antibacterial drug, which is widely used in clinical practice. Norfloxacin antibiotics have very good inhibitory activity against most Gram-positive bacteria, E. Cocci (especially group D streptococci), enterococci and anaerobic bacteria have little or no inhibitory activity. With the wide application and in-depth research of this class of drugs, there are more and more reports on the adverse reactions and drug resistance of norfloxacin drugs, and its potential serious adverse reactions have gradually attracted people's attention. It is used for animals, so the possibility of its residue in animal edible products is relatively high. These residues can directly cause ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N1/28G01N30/08G01N30/36G01N30/72
Inventor 张雪峰崔涛常建军刘卫星
Owner INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD
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