biocommaIntroduction
Coffee, a daily beverage, is highly reliant on quality and safety.Mycotoxin contamination, notably Ochratoxin A (OTA), is a keyrisk factor affecting coffee quality. Biocomma established aUPLC-MS/MS method for detection of OTA by Copure® MAXCartridges with good recovery and precision for your reference.The recoveries were 95-105% with RSD less than 5%.
Experiment
Extraction
Weigh 2.50 g of ground coffee bean into a 50 mL centrifugetube. Add 25 mL of 30 g/L methanol-sodium bicarbonatesolution (50:50, v/v). Vortex for 10 min. Centrifuge at 8000 r/min for 5.0 min, then filter the supernatant with filter paper.Collect 10 mL of the extracted filtrate for purification.
Purification (Copure® MAX Cartridge, 200 mg/ 3 mL)
Activation: activate the Copure® MAX Cartridge by 5 mL ofmethanol, then 5 mL of 30 g/L methanol-sodium bicarbonate(50:50, v/v).
Loading: add the prepared solution at flow rate of 1~2 drop/s.Drain the cartridge.
Washing: wash the cartridge by 5 mL of washing solution (0.1mol/L potassium hydroxide: acetonitrile: water = 3:50:47, v/v),5.0 mL of water, and 5.0 mL of methanol sequentially. Drain thecartridge.
Elution: add 5 mL of eluent solution (methanol: acetonitrile:formic acid: water = 40:50:5:5, v/v). Collect the eluateand evaporate to nearly dryness at 45 ℃ . Add 1.0 mL ofacetonitrile-2% acetic acid aqueous solution (50:50, v/v), andvortex to reconstitute. After filter into a sample vial, the sampleis ready for analysis.
Preparation of Procedural Blank
Carry out the experiment according to the above steps withoutsample.
Instrumental Conditions
Instrument: Thermo Scientific UltiMate 3000
Chromatographic column: Commasil® AQ-C18 (4.6 mm*250mm, 5 um)
Detector: FLD (excitation wavelength 333 nm, emissionwavelength 460 nm)
Mobile phase: A: 2% acetic acid water, B: acetonitrile
Flow rate: 1 mL/min
Injection volume: 5 µL
Table 1. Gradient Elution Program
Results
Table 2. Spiked Ochratoxin A In Coffee Bean Recovery
Ordering Information
