Lcq deca mass spectrometer

The contents of the identified phenolic compounds in the olive leaves were quantified using a HPLC-DAD-MS system. The polyphenols were separated using a Shimadzu LC-2030C HPLC system (Kyoto, Japan) coupled with a ZORBAX SB-C18 column (4.6 × 250 mm², 5 μm, Agilent Technologies, Savage, MD, United States), and the mobile phases were 1% acetic acid in deionized water (mobile phase A) and acetonitrile (mobile phase B). The following elution conditions were used: 0–11 min, 10%–25% B; 11–16 min, 25%–28.5% B; 16–40 min, 28.5%–90% B; 40–50 min, 90% B; 50–55 min, 90%–10% B; 55–60 min, 10% B, and the flow rate was 1 mL/min. A Thermo Finnigan LCQ DECA mass spectrometer, equipped with an electrospray source, was used for detection, and analyses were performed with scans from 125 to 1,200 m/z in negative and positive ion modes. The peaks were identified using an Xcalibur Qual browser, and the quality data and relative retention times of the identified phenolic compounds were compared by UHPLC-Q-Exactive Orbitrap-MS. Then, the spectral peaks were quantitatively analyzed with LabSolutions HPLC software, using calibration curves of the corresponding standard or a compound that contained a similar aglycone (Supplementary Table 1).

Electron spray ionization mass (ESIMS) was recorded on an LCQ DECA mass spectrometer (Thermo Finnigan, Bremen, Germany) coupled with an Agilent 1100 HPLC using photodiode array detector. NMR spectra were recorded on a Bruker DRX-400 MHz Ultrashield spectrometer (Bruker BioSpin, Billerica, MA, USA). CD₃OD was used as a solvent, and TMS as the internal reference. Pre-coated thin layer chromatography (TLC) plates; Silica gel 60 F₂₅₄ were purchased from Merck, Darmstadt, Germany. Silica gel 60 (70–230 mesh), Diaion HP-20, and polyamide 6 (Merck, Darmstadt, Germany) were used for different column chromatographic procedures.

A UV spectrum was accomplished utilizing a Hitachi-300 spectrometer (Hitachi High-Technologies Corporation/Kyoto/Japan). An ESIMS was performed with a LCQ-DECA mass spectrometer (Thermo_Finnigan/Bremen/Germany). An HRESIMS was executed utilizing a Micromass_Qtof2 spectrometer (Bruker/Rheinstetten/Germany). NMR spectra were determined on BRUKER_AVANCE600 equipment (BioSpin-Bruker/Billerica/MA/USA). IR data were estimated with an Infrared-400 Shimadzu spectrophotometer (Shimadzu/Kyoto/Japan). A chromatographic investigation was carried out on SiO₂ 60 (0.04–0.063 mm)/Sephadex LH-20 (0.25–0.1 mm)/RP-18 (0.04–0.063 mm) (Merck/Darmstadt/Germany). Precoated SiO₂60_F₂₅₄ TLC plates (0.2 mm, Merck/Darmstadt/Germany) were employed for TLC examination. The metabolites’ purification and detection were carried out by employing a LiChrolut_RP-18 6 mL solid-phase extraction tube and UV inspection at λ_max 366 and 255 nm and then spraying with H₂SO₄: p-anisaldehyde and a 110 °C heating.

MS analysis was performed on a Thermo LCQ Deca mass spectrometer. The experiments were performed using negative ionization mode with a spray voltage of 3 kV and a capillary temperature of 275 °C [33 (link)]. MS data were acquired and processed using Xcalibur 1.3 software.

The FT-IR spectra of the sample were assessed in the range of 400–4000 cm⁻¹ with KBr discs, compared to authentic CPT. The extracted CPT samples were dissolved in CHCl₃, and their structural identity was resolved by ¹HNMR (JEOL, ECA-500II), the chemical shifts (δ-scale) and coupling constants (Hz) were expressed by ppm [13 (link), 14 (link), 29 (link)].
The chemical identity of the extracted CPT was resolved by LC–MS/MS (Thermo Scientific LCQ Deca mass spectrometer equipped with an electrospray source) [11 (link), 13 (link), 14 (link), 22 (link), 29 (link)]. The ion trap was scanned from 300 to 2000 m/z, and the mass scan was recorded at 300 to 2000 Da. The structure of the compound was identified based on their mass spectral fragmentations and retention time by NIST mass spectral library [29 (link), 41 (link)].

NMR experiments were carried out on a Bruker AVIII 600 MHz NMR spectrometer (Bruker BioSpin GmbH company, Rheinstetten, Germany) (¹H 600 MHz, ¹³C 150 MHz), with tetramethylsilane as the internal standard. Optical rotations were recorded with an MCP 300 (Anton Paar, Shanghai, China) polarimeter at 28 °C. UV spectra were measured on a PERSEE TU-1900 spectrophotometer. IR spectra were carried out on a Nicolet Nexus 670 spectrophotometer, in KBr discs. CD spectra were measured on a Chirascan™ CD spectrometer (Applied Photophysics, London, UK). ESIMS spectra were recorded on a Finnigan LCQ-DECA mass spectrometer, and HRESIMS spectra were recorded on a Thermo Fisher Scientific Q-TOF mass spectrometer. Column chromatography (CC) was performed on silica gel (200–300 mesh, Qingdao Marine Chemical Factory, Qingdao, China) and Sephadex LH-20 (Amersham Pharmacia Biotech., Uppsala, Sweden). Thin-layer chromatography (TLC) was performed on silica gel plates (Qingdao Huang Hai Chemical Group Co., Qingdao, China, G60, F-254). The high-performance liquid chromatography (HPLC) separation was performed on a Varian Prostar 210 system equipped with a Prostar 320 UV detector on a preparative Hypersil C-18 BDS column (250 × 21.2 mm, L × ID, 5 μm Varian Dynamax, Thermo Fisher Scientific Inc., Waltham, MA, USA). All other chemicals used were analytical grade.