biocommaExperiment
Extraction
Weigh 5 g of honey into a 50 mL centrifuge tube, add 10 mLof water. Vortex for 1 min. Add 20 mL of n-hexane-acetonesolution (1:1), and vortex for 3 min. Centrifuge at 9500 r/min for 5 min, and transfer the upper layer to a 150 mLflask. Repeat the extraction once with 20 mL of n-hexaneacetone solution (1:1). Combine the extracted solution, andconcentrate in a water bath at 40 °C under reduced pressureto nearly dryness. Add 3 mL of n-hexane to dissolve and setaside.
Purification(Copure® Florisil SPE Cartridge, 1000 mg/ 6 mL)
Activate the Copure® Florisil SPE Cartridge by 5 mLof n-hexane-acetone solution (95:5), then 5 mL ofn-hexane. Pipette the prepared solution to the cartridge.Wash the flask with 3 mL of n-hexane, and transfer tothe cartridge. Elute with 10 mL of n-hexane-acetonesolution (95:5).
Collect the eluate and evaporate to nearly dryness at 40℃ . Reconstitute with 1.0 mL of n-hexane. The sampleis ready for analysis.
Instrumental Conditions
Instrument: Gas Chromatograph (Agilent 7890B)
Chromatographic column: Agilent Technologies DB-35MSUI (30 m×0.250 mm, 0.25 µm)
Carrier gas: nitrogen (purity ≥ 99.999%)
Injection port temperature: 280 ℃
Detector temperature: 300 °C
Column temperature: The initial column temperature is 80°C, and maintain 1 min. Raise to 220 °C at a rate of 40 °C/min, and maintain 1 min. Then, raise to 300 °C at a rate of10 °C/min, and maintain 1.5 min.
Carrier gas flow:1.2 mL/min
Injection volume: 1 µL
Injection method: splitless injection
Results
Table 1. Fluvalinate Spiked Recovery in Honey at 10 μg/kg
Ordering Information
