biocommaExperiment
Extraction
Weigh 5 g of ground chicken into a 50 mL centrifuge tube.Add 15mL 1% trichloroacetic acid/acetonitrile (15+85, V/V),homogenize at high speed for 5min. Centrifuge at 9500r/minfor 5min, and then pipette the supernatant into a 100 mLseparatory funnel.Add 10 mL of 1% trichloroacetic acid/acetonitrile (15+85,V/V) to the residue. Repeat step 1. Combine the extracts.Add 30 mL of n-hexane and shake for 2 min. After settleinto layers, collect the lower layer into a flask. Evaporateto approximately 1 mL at 40 °C in a water bath. Transfer toa 10 mL centrifuge tube. Rinse the flask with 2 mL of 1%trichloroacetic acid/acetonitrile (15+85, V/V), then 2 mL of0.1 mol/L hydrochloric acid. Centrifuge the combined liquidsat 9500 r/min for 5 minutes. The supernatant is ready forpurification.
Purification (Copure® MCX Cartridge, 60 mg/ 3 mL)
Activation: activate the Copure® HLB Cartridge by 3mLmethanol, then 3 mL of 0.1 mol/L hydrochloric acid.
Loading: add the prepared solution to the activatedcartridge.
Washing: wash the cartridge by3 mL of 0.1 mol/L hydrochloric acid, then 3 mL of methanol. Drain thecartridge.
Elution: add 5 mL of 5% ammoniated methanol. Collect allthe eluate. Evaporate sample to near dryness at 40 ℃ . Add 1 mL of mobile phase. After filter by 0.22 μm membrane, thesample is ready for analysis.
Preparation of Standard Curve Solution
Dilute cyromazine standard working solution with mobilephase to prepare series of standard concentrations of 0.05μg/mL, 0.1 μg/mL, 0.2 μg/mL, 0.4 μg/mL, 0.8 μg/mL, 1.0 μg/mL, 2.0 μg/mL.
Instrumental Conditions
Instrument: Liquid Chromatograph (1260 Infinity II, with UVdetector)
Chromatographic column: Infinity Lab Poroshell 120 HILIC,2.1 x 100 mm, 2.7 μm
Mobile phase: 25 mmol/L ammonium acetate solutionacetonitrile (40+960, V/V)
Flow rate: 0.300 mL/min
Detection wavelength: 214 nm
Column temperature: 30 ℃
Column temperature: 30 ℃
Results
Table 1. Cyromazine Spiked Recovery in Chicken at 0.080mg/kg
Figure 1. Chromatogram of Cyromazine Standard Solution (0.500 μg/mL)
Ordering Information
