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Liquid quality method for rapid screening and detection of 102 veterinary drug residues in poultry and livestock meat
Date: 2025-06-19Read: 16

This study addresses the issue of multiple veterinary drug residues in animal derived foods using ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)Technology has established a fast and accurate method for detecting multiple residues. This method has high sensitivity and selectivity, and has been successfully applied to actual sample detection, providing a powerful tool for food safety supervision.

based onFaVEx-NMPurification column and ultra-high performance liquid chromatographyseries connectionmass spectrometryUPLC-MS/MSTechnology has been developed to simultaneously detect substances in animal derived foods102Residues of veterinary drugsRapid screening and testing methodsBy optimizing the extraction solvent and purification method, the extraction efficiency of the target compound has been improved. At the same time, the chromatographic and mass spectrometry conditions were evaluatedoptimizeenhanceimproverefineThis ensures the sensitivity and accuracy of the method. The detection limit and quantification limit of this method have respectively reached0.04~2.2 μg/kg70 and 0.09~4.4 μg/kgThe recovery rate remains stable at%~120%Relative standard deviation1.34 RSD)In%~10.97

%between.The types of veterinary drugs tested in this article include13Sulfonamides102β -Xingxing stimulants, quinolones, macrolides, tetracyclines, nitroimidazoles, glucocorticoids, steroids, tranquilizers, antiviral drugs, chloramphenicol, quinolones and metabolites, fipronil and metabolitescategoryResidues of veterinary drugs. Actual inspectionSample Typeincluding3Pork and beef

and

chicken

Seed.

(1) The reagents, consumables, and equipment are as follows:

material

Specifications

acetonitrile

chromatographically pure

methanol

Chromatographic pure Chun

Glacial acetic acid

Superior purityformic acid

Mass spectrometry levelFaVEx-NMSolid phase extraction columnUniversal

SPE

pillar

, 50/PK

Needle filter membrane filter head

0.22 μm

Acquity UPLC BEHC18

100 mm×2.1 mm×1.7 μmInstrument name

manufacturerQTRAP 5500+Liquid chromatography-mass spectrometer

the United StatesAbout SCIEX

Co., Ltd.ME802EType analysis balance

Teller

-

Toledo Instruments (Shanghai) Co., LtdUltrapure Water System

Sadolis Scientific Instruments Co., Ltd

Hand simulation

oscillator

Juyan Technology Co., Ltd

Positive pressure column pressJuyan Technology Co., Ltdpipette gun

France

GilsoncompanyVortex Mixer

Germany

Th5 company(2) Sample pretreatment method50 Weigh outgMeat samples2mL4In the centrifuge tube, add5g NaSO2Water purifying agent, homogeneous proton, oscillation5 minAdd to include%V/VAcetonitrile solution of acetic acid10 mLAs an extraction solution, mix well and shake15 min.6000 r·mincentrifugation5 minTake the supernatant5 mL1passFaVEx-NMPurification column, positive pressure purification, flow rate per second

Drip out, collect all purified liquid, pass through

0.22 μm

Perform machine testing after filtering the membrane.(3) Chromatography and mass spectrometry conditions (omitted here, please feel free to contact and request if needed)(4) The linearity, detection limit, and quantification limit of the method0In order to eliminate the influence of matrix effects on quantitative determination, this experiment used a standard paired curve for quantification. Taking pork as an example, a standard working solution was prepared using blank pork extract. according to0.5“2.3”1.0The method for handling the concentration gradient of standard working solution is as follows:5.010.020.0-1The50.0 ng·mLThe matrix spiked solution, according tomass spectrometryTest the conditions and take the concentration of the standard working solution of the spiked matrix as the horizontal axisx, vertical axisy2To quantify the ion peak area, obtain the standard matrix curve, linear regression equation, and correlation coefficientRRefer to the national standardGB/T 33260standard method[121]The detection limit of the calculation methodLODAnd quantitative limitLOQ

, result

Welcome to request.

List of validated drugs in this article (contact to request recovery rate data)

Sulfapyridine

Tuobutro

地塞米松

Sulfadiazine

Zipatero

Dexamethasone acetate

Sulfathiazole

Marvelo

Fluorometholone

Sulfamethoxazole

Norfloxacin

QunbolongTrimethoprimEnrofloxacin

Nuolong(

19-

Nortestosterone)

Sulfonamide trimethoprim

Sparfloxacin

Methyltestosterone

Sulfamethoxazole pyridazine

Florfenicol

Progesterone (Progesterone)

Sulfamethoxazole

Peofloxacin

Testosterone propionate

SulfamethoxazoleOfloxacinDiDi Zepam

sulfonamide

-6-

Methoxypyrimidine

Enrofloxacin

Triazolam

Sulfobenzoyl

Ciprofloxacin

Chlorpromazine

Sulfamethoxazole

Lomofloxacin

Midazolam

Sulfoquinoxaline

Dafloxacin

Laolao Rasipam

Sulfamethoxazole

Quinic acid

Amantadine

Sulfamethoxazole

Sinofloxacin

Jingang ethylamine

Sulfamethoxazole

Naphthalene acid

QuinqueethanolSulfamethoxazole吡哌酸3-

Methyl quinoxaline

-2-

carboxylic acid

Sulfamethoxazole

Roxithromycin

Chloramphenicol

Sulfamethoxazole

Timikau Star

Florfenicol

Sulfamethazine

Clindamycin

Fluoronitrile

Sulfamethoxazole

Tylosin

Fluconazole sulfone

Bambutro

erythromycin

Fipronil sulfide

Brombuterol

Lincomycin

Dikezhuli

Xibutuo

tetracycline

Qu'an Xilong

Clenbuterol

Oxytetracycline

Azithromycin

Chlorpheniramine

Chlortetracycline Chlorolv nitrogen level

Mabuturo

Doxycycline

(Doxycycline)

Zolpidem

Ractopamine

Hydroxymetronidazole

Ai Si zolam

Hydrocortisone

Metronidazole

Titimazepam

Methylprednisolone

Dimetridazole

Go to Qujiaxipan

betamethasone

Luonidazole

Difluoroxacin

Fluhydrocortisone acetate

Benzimidazole

Salafloxacin

Difukete

Isopropyl nitroimidazole

Enrofloxacin

cortisone



Prednisone

MabofloxacinBenba Ba Bituo(5) Accuracy and precision13To verifyFaVExOne step purification method for determination1Accuracy of veterinary drug residues, validation of spiked recovery rate for negative samples that have been tested.3Three different levels of addition were used(μg/kg5Theμg/kgTheμg/kg), andmakeuseFaVEx-NM6Purification columnfrontProcessing, parallel measurementSample, repeat three times, calculate the average relative standard deviation(RSD)And the recycling rate. The experimental results are shown in the table12-670.16 In μg/kgThe average recovery rate of adding levels is%~112.87%2.96 RSDfor3.0%~10.97%70.54 In μg/kgThe average recovery rate of adding levels is%~119%1.34 RSDfor5.0%~10.75%69.9 In.27 μg/kgThe average recovery rate of adding levels is%~109%1.73 RSDfor

%~10.44

%.