Application of UHPLC-ESI-Q-TOF-MS to Identify Multiple Constituents in Processed Products of the Herbal Medicine Ligustri Lucidi Fructus

Abstract

Ligustri Lucidi Fructus (LLF), the fruit of Ligustrum lucidum Ait. (Oleaceae), has been used as a common herbal medicine in clinical practice in China for nearly 2000 years. In most cases, LLF is prescribed in decoctions in the form of processed products rather than crude drugs. In this study, an ultra-high performance liquid chromatography coupled with electrospray ionization-quadrupole-time of flight-mass spectrometry (UHPLC-ESI-Q-TOF-MS) method was established for rapid separation and identification of multiple constituents in the 80% methanol extract of processed-LLF. A total of 50 compounds (one phenylethanoid, seven phenylethanoid glycosides, seven flavonoids, 25 iridoids, nine triterpenoids and one cyclohexanecarboxylic acid) were either unambiguously identified or tentatively characterized with the aid of authentic standards or published data. Luteolin-7-O-rutinoside, oleoside and secologanoside were detected in LLF for the first time. This study enriches the chemical profiling of processed-LLF and could provide valuable information for the quality control and further investigation of processed-LLF and crude LLF.

Systematic Profiling of the Multicomponents and Authentication of Erzhi Pill by UHPLC/Q-Orbitrap-MS Oriented Rapid Polarity-Switching Data-Dependent Acquisition and Selective Monitoring of the Chemical Markers Deduced from Fingerprint Analysis

“…In the case of an unknown iridoid compound ( 4 # in Table S2; t R 4.29 min), (Figure 4), the precursor ions in ESI− ( m / z 375.1306) and ESI+ ( m / z 399.1257) could infer the molecular formula C 16 H 24 O 10 . Diverse product ions in the negative mode, m / z 331.1407 ([M-H-CO 2 ] − ), 287.1507 ([M-H-CO 2 -CH 3 CHO] − ), 195.0666 ([M-H-Glc-H 2 O] − ), together with two positive fragments m / z 355.1358 ([M + Na-CO 2 ] + ) and 203.0526 ([Glc + H 2 O + Na] + ), could infer the structure of loganic acid [23]. We could finally characterize 35 iridoid compounds from EZP, and six of them ( 28 #: ligulucidumoside C: 39 #: oleuropeinic acid; 46 #: specnuezhenide; 65 #: oleonuezhenide; 70 #: 6′- O - trans -cinnamoyl-8-epikingisidic acid; 75 #: ligulucidumoside A; Table S2) had been confirmed with the aid of reference compounds.…”

“…For the unknown phenylethanol compound 14 # (t R 5.48 min), a pentose ( m / z 299.1155 for [M-H-pentose] − and 323.1101 for [M + Na-pentose] + ) and a hydroxyphenylethanol group ( m / z 121.0648) attached to Glc could be characterized (Figure 4). Accordingly, we could characterize compound 14 # as osmanthuside H (or isomer) [23].…”

Analgesic, Anti-Inflammatory, Cytotoxic Activity Screening and UPLC-PDA-ESI-MS Metabolites Determination of Bioactive Fractions of Kleinia pendula

“…Significantly, the hexane fraction showed the most potent cytotoxic effect against all the cancer cell lines tested. The UPLC-PDA-ESI-MS metabolite screening of bioactive hexane fraction revealed the presence of major metabolites including tormentic acid [34], 5-hydroxyadvisiosidec [36], citrostadienyl [37], dehydrated derivative of tinosposinenside B [30] and tinocrisposide [30]. The observed cytotoxic activity could be attributed to the presence of fatty acids and triterpenoid (tormentic acid [47]) in the hexane fraction.…”

Natural Deep Eutectic Solvent as Extraction Media for the Main Phenolic Compounds from Olive Oil Processing Wastes

“…This feature helped in the complete identification of the compounds and in the differentiation between the isobaric compounds. The ability of HPLC-ESI-QTOF-MS for qualitative identifications has been reported in several studies [48][49][50].…”