HPLC Analysis of Grapefruit Juice on Ascentis^® Express C18 Column

sample preparation

SPE (Solid Phase Extraction)

sample/matrix

grapefruit juice hand-squeezed in laboratory, centrifuged and filtered through a 0.45 μm nylon filter disc (Acrodisc)

column

Ascentis Express C18, 5 cm x 4.6 mm I.D., 2.7 μm particles (53826-U)

mobile phase

[A] water/formic acid (99.9:0.1); [B] water/acetonitrile/isopropanol/formic acid (39.9:20:40:0.1)

gradient

10% B for 3 min; 10 to 34% B in 30 min; 34 to 100% B in 1 min; held at 100% B for 6 min; 100 to10% B in 1 min

flow rate

0.8 mL/min

column temp.

ambient

detector

PDA: 190–370 nm; chromatogram extracted at 283 nm

detector

ESI-MS: mass spectral range, 250-700 m/z; interval, 0.5 s; scan speed, 938 amu/s; nebulizing gas (N2) flow, 1.5 L/min; interface temperature, 350 °C; (heat block, 300 °C; desolvation line (DL) temperature, 300 °C; DL voltage, 34 V; probe voltage, +4.5 kV; Qarray voltage, 1.0 V; RF voltage, 90 V; detection gain, 1.05 kV.)

injection

2 μL