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Method for determining aminoglycoside drug in animal muscle tissue without using of ion pair reagent

A technology of aminoglycosides and ion-pair reagents, which is applied in the field of determination of aminoglycosides in animal muscle tissue without using ion-pairing reagents, and can solve problems such as difficult reversed-phase column retention, human hazards, and residues of aminoglycosides

Inactive Publication Date: 2018-08-31
SOUTH CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, such drugs have side effects such as ototoxicity and nephrotoxicity. Continuous use and unreasonable use will lead to excessive residues of aminoglycosides in food animals, causing potential harm to humans through the food chain
[0003] At present, domestic and foreign reports on the detection methods of aminoglycosides in animal-derived foods mainly include liquid chromatography-tandem spectrometry, etc., but due to the high polarity of aminoglycosides, it is difficult to use traditional reversed-phase chromatography Therefore, ion-pair reagents need to be added to the mobile phase to enhance chromatographic retention
However, the use of ion-pair reagents will not only cause irreversible damage to the chromatographic column, but also cause serious ion suppression and corrosion of the ion source

Method used

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  • Method for determining aminoglycoside drug in animal muscle tissue without using of ion pair reagent
  • Method for determining aminoglycoside drug in animal muscle tissue without using of ion pair reagent
  • Method for determining aminoglycoside drug in animal muscle tissue without using of ion pair reagent

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preparation example Construction

[0072] In the present invention, the preparation method of the described sample injection includes:

[0073] 1) Mix the animal muscle tissue with the phosphate extract, perform the first ultrasonic treatment for 8-12 minutes to obtain the first ultrasonic treatment product, and centrifuge the first ultrasonic treatment product to obtain the first precipitate and the first clear liquid ;

[0074] 2) Mix the first precipitate obtained in step 1) with the phosphate extract, perform the second ultrasonic treatment for 8 to 12 minutes to obtain the second ultrasonic treatment product, and centrifuge the second ultrasonic treatment product to obtain the second ultrasonic treatment product. Second precipitation and second clear solution;

[0075] 3) mixing the first clear liquid obtained in step 1) with the second clear liquid obtained in step 2) to obtain a mixed clear liquid;

[0076] 4) Add the mixed clear liquid obtained in step 3) into the MCX column, rinse with acetic acid so...

Embodiment 1

[0105] The percentage concentration of the solution involved in this embodiment is volume percentage concentration unless otherwise specified.

[0106] 1. Preparation of standard solution

[0107] Precisely weigh 10 mg each of neomycin B, apramycin, kanamycin B, tobramycin, vertamycin, hygromycin B, gentamicin, amikacin, and spectinomycin, Dilute the volume in a 10mL brown volumetric flask with ultrapure water and mix well to obtain a standard stock solution with a concentration of 1mg / mL for each drug, and dilute it with ultrapure water to form a mixed standard working solution with an appropriate mass concentration, -20°C Store away from light, valid for 1 month.

[0108] 2. Preparation of phosphate extract

[0109] Accurately weigh 1.36 g of potassium dihydrogen phosphate, dissolve it in 980 mL of water, add 0.15 g of disodium edetate and 20 g of trichloroacetic acid in sequence, fully dissolve and mix, and dilute to 1 L with ultrapure water.

[0110] 3. Sample Preparati...

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Abstract

The invention provides a method for determining an aminoglycoside drug in an animal muscle tissue without using of an ion pair reagent, and belongs to the technical field of veterinary drug residue detection, and the method comprises performing liquid chromatography-tandem mass spectrometry detection on an injection sample, and obtaining the content of the aminoglycoside drug in the injection sample according to a standard curve of the content of the aminoglycoside drug and a liquid chromatogram of the injection sample; wherein a liquid chromatography column is SIELC Obelisc R. The method provided by the invention can enhance the chromatographic retention without using of the ion pair reagent, and can detect the content of the aminoglycoside drug the animal muscle tissue, the detection limit and the limit quantification of the drug are respectively in a range of 1 to 10 mu g / kg and a range of 2-20 mu g / kg; within-run precision and between-run precision are 2-14.4% and 3.7-19.8% respectively.

Description

technical field [0001] The invention belongs to the technical field of detection of veterinary drug residues, and in particular relates to a method for determining aminoglycoside drugs in animal muscle tissue without using ion-pair reagents. Background technique [0002] Aminoglycoside antibiotics are a class of broad-spectrum antibiotics, which have significant inhibitory effects on both Gram-negative and Gram-positive bacteria. They are widely used in the treatment of various animal diseases, and are often added to feed for Promote animal growth and development. However, such drugs have side effects such as ototoxicity and nephrotoxicity. Continuous use and irrational use will lead to excessive residues of aminoglycosides in food animals, causing potential harm to humans through the food chain. [0003] At present, domestic and foreign reports on the detection methods of aminoglycosides in animal-derived foods mainly include liquid chromatography-tandem spectrometry, etc....

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N30/72G01N2030/146
Inventor 贺利民李玖锋曾振灵刘戎苏贻娟
Owner SOUTH CHINA AGRI UNIV
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