Lcq advantage spectrometer

The individual ellagitannin composition was also determined. The equipment used for this analysis was a Thermo-Finnigan Surveyor HPLC system composed of a Surveyor PDA plus detector, a Surveyor autosampler, and Surveyor a quaternary pump controlled by Xcalibur data treatment system. This HPLC system was also coupled to a Thermo-Finnigan LCQ Advantage spectrometer equipped with an ion trap mass analyzer. The electrospray ionization mass spectrometry detection was realized in negative ion mode with the below optimized parameters: capillary temperature 400 °C, capillary voltage 3 V, nebulizer gas flow 1.75 L/min, desolvation gas flow 1 L/min, and spray voltage 5 kV. The analyses were accomplished in duplicate on a 250 × 4.6 mm, 5 μm Lichrospher 100 RP 18 column. The mobile phases applied were solvent A [water/formic acid (99.6/0.4)] and solvent B [methanol/formic acid (99.6/0.4)]. The gradient elution was 0–3% B in 5 min, 3–12% from 5 to 35 min, and 12–100% from 35 to 40 min with a flow rate fixed at 1 mL/min and a detection wavelength maintained at 280 nm. Each ellagitannin was quantified via its molecular ion, based on external calibration curve of castalagin standard and the results are expressed as equivalents of castalagin.

Electrospray ionization mass spectra (ESI-MS) were recorded on a Thermo Finnigan LCQ Advantage spectrometer (Hemel Hempstead, Hertfordshire, UK). Mass spectra acquisition was performed in positive and negative ion mode in a mass range of 50–2000 m/z. Source parameters: T, 200 °C; sheath gas flow rate, 20 arb; aux gas flow rate, 10 arb; spray voltage, 5.50 kV; capillary temperature, 275 °C; capillary voltage, 38.00 V; tube lens, 65.00 V.
Electrospray ionization high-resolution mass spectrometry (ESI-HR-MS) analyses were performed on a Synapt G2-Si QTof instrument (Waters, Milford, MA, USA) equipped with a ZsprayTM ESI-probe for electrospray ionization (Waters, Milford, MA, USA). The sample was dissolved in water–0.1% formic acid in methanol and analyzed by direct infusion. The ion source and interface conditions were as follows: capillary voltage 1.3 kV, sampling cone 120 V, source temperature 120 °C, desolvation temperature 150 °C and desolvation gas flow rate 600 L h⁻¹. Mass spectra were acquired over the m/z range 50–1000 in a positive ion Full Scan mode. Leucine enkephalin was used as a lock-mass compound. Data were processed with MassLynxTM V4.2 software (Waters Milford, MA, USA).