Rapid identification and determination of 11 polyphenols in Herba lycopi by HPLC–MS/MS with multiple reactions monitoring mode (MRM)

A new and rapid method was developed for simultaneous identification and determination of 11 polyphenols in Herba lycopi, i.e. rosmarinic acid, protocatechuic aldehyde, protocatechuic acid, caffeic acid, ferulic acid, apigenin, luteolin, quercetin, isorhamnetin, chlorogenic acid and rutin, using high performance liquid chromatography (HPLC) coupled with triple quadrupole mass spectrometry (MS/MS). Quantitation was based on multiple reactions monitoring (MRM) using the precursor → production combination for the determination of 11 analytes. The analysis was performed on an Eclipse Plus C18 column (I.D. 4.6 mm × 100 mm, 3.5 μm particle size). An electrospray ionization (ESI)-tandem interface in the negative mode was employed prior to mass spectrometric detection. With the optimized conditions, the 11 biomarkers were detected properly within 3 min. Limits of detection (LOD) ranged from 0.6 to 2.6 ng/ml. The average recoveries ranged from 95.42 to 101.11% with RSDs ≤ 2.23%. The applicability of this analytical approach was confirmed by the successful analysis of 3 samples. The established method was validated and found to be sensitive and reliable for the determination of 11 analytes in Herba lycopi.