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Green Giant Research Technology Trading (Shanghai) Co., Ltd
ada@getc.com.cn
Room 609, 6th Floor, Hongmei Business Building, 8075 Humin Road, Xuhui District, Shanghai
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 spectrometry(UPLC-MS/MS)Technology 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/V)Acetonitrile 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:5.0、10.0、20.0、、-1、The50.0 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 axis(x), vertical axis(y)2To quantify the ion peak area, obtain the standard matrix curve, linear regression equation, and correlation coefficient(R)Refer to the national standardGB/T 33260standard method[121]The detection limit of the calculation method(LOD)And quantitative limit(LOQ
) | ||
, 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 table12-6,70.16 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
%.