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11.
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1 Scope of application
This method is suitable for honey fourteen kinds of quinolone ( enoxacin , norfloxacin , marbofloxacin , FLEROXACIN , ciprofloxacin , ofloxacin , danofloxacin , enrofloxacin , Austria ratio of gatifloxacin , sarafloxacin , sparfloxacin , difloxacin , oxolinic acid , flumequine ) residues liquid chromatography - tandem mass Spectrometry
.
The detection limits of the fourteen quinolone methods are all 2ug/kg
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2 Principle of the method
Quinolone residues in honey are extracted with phosphate buffer solution (pH=3), filtered, purified by Oasis HLB or equivalent solid phase extraction column, eluted with ammonium hydroxide methanol solution and evaporated to dryness, and the residue is used with constant volume solution After dissolving and passing through a 0.
2um filter membrane, the sample solution is measured by a liquid chromatography-tandem mass spectrometer and quantified by an external standard method
.
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2.
3 Reagents and materials
Acetonitrile, methanol (HPLC grade, Dima), phosphoric acid, acetic acid, ammonium hydroxide, potassium dihydrogen phosphate, dipotassium hydrogen phosphate (excellent grade pure, Tianjin Chemical Reagent Second Plant), enoxacin, norfloxacin , Mabofloxacin, Fleroxacin, Ciprofloxacin, Ofloxacin, Danofloxacin, Enrofloxacin, Orbifloxacin, Sarafloxacin, Sparfloxacin, Difloxacin, Umolinic Acid , Fmequine standard (sigma-aldrich company in Germany), Oasis HLB solid phase extraction column (500mg/6mL, waters company in the United States), water is high purity water
.
Phosphate buffer solution: 0.
Quinolone standard stock solution: 1mg/mL
.
Accurately weigh an appropriate amount of each quinolone standard substance, and use ammonium hydroxide methanol solution to prepare a 1mg/mL standard stock solution.
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4 Instruments and equipment
API 3000 liquid chromatography-tandem quadrupole mass spectrometer, equipped with electrospray ion source (AB company in the United States), 1100 liquid chromatograph (Agilent company in the United States), TurboVapLV nitrogen concentrator (Caliper company in the United States), 550ApH meter (United States ThermoOrion), MilliQ deionized water generator (Millipore, USA), VORTEX-2 vortex mixer (Scientific Industries, USA)
.
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2.
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5 Sample preparation
(1) Extraction
Weigh 5g of the sample (accurate to 0.
01g), place it in a 150mL Erlenmeyer flask, add 30mL of 0.
05mol/L phosphate buffer solution (pH=3), and mix quickly on a liquid mixer for 1 min to make the sample complete Dissolve
.
(2) Purification
Connect the glass reservoir plugged with glass wool to the OasisHLB solid phase extraction column, pour the sample liquid into the glass reservoir, adjust the flow rate ≤ 3mL/min to make the sample liquid pass through the OasisHLB solid phase extraction column, and wait until the sample solution is complete After flowing out, wash the column with 5 mL water and 5 mL methanol+water (3+7) respectively, and discard all the effluent
.
The solid phase extraction column was drained under a negative pressure of 65 kPa for 30 min, and then eluted with 5 mL of ammonium hydroxide methanol solution (1+19).
According to the above-mentioned extraction and purification operation steps, a sample blank extract solution for preparing a series of matrix standard working solutions is prepared
Related links: Repeatability and reproducibility of 15 quinolone drug residue determination methods in eel and its products