Avance 2 400 nmr spectrometer

The FTIR spectra were obtained by means of a FTIR-4000 instrument (JASCO, Tokyo, Japan) and peaks were given in terms of wave number (cm⁻¹). The ¹H-NMR and ¹³C-NMR spectra of the synthesized compounds were recorded on an Avance II 400 NMR spectrometer (Bruker, Biospin AG Industriestrasse 26, CH-8117, Fallanden, Switzerland)at 400/100 MHz frequency in CDCl₃ and using TMS as internal standard (chemical shift δ in ppm). The ³¹P-NMR spectra of compounds were recorded in CDCl₃ using phosphoric acid (H₃PO₄) as external standard (chemical shift δ in ppm). The mass spectra were executed on a Micromass Q-Tof system (Waters, UK). Elemental analyses were done with a FLASHEA 112 analyzer (Shimadzu, Mumbai, Maharashtra, India) and all analyses were consistent (within 0.4%) with theoretical values. A Vibra Cell VCX-500 ultrasound synthesizer (Sonics, Newtown, CT, USA) equipped with a solid probe was employed for the synthesis of intermediate 1. In vitro anti-cancer activity screening of the synthesized compounds was accomplished at the Anti-Cancer Drug screening facility (ACDSF) at ACTREC (Tata Memorial Centre, Navi Mumbai, India).

All the chemicals required for experiments were of analytical grade and were purchased from Loba Chemie (Mumbai, India), SRL (Mumbai, India), and Sigma Aldrich (Germany). Nutrient agar, nutrient broth, sabouraud dextrose agar and sabouraud dextrose broth required for antimicrobial and preservative efficacy were obtained from Hi-media Laboratories. Streptomycin, ciprofloxacin, ampicillin and fluconazole were obtained as gift sample from Belco Pharma, Bahadurgarh, India. Microbial strains S. aureus MTCC 3160, P. aeruginosa MTCC 1934, E. coli MTCC 45, C. albicans MTCC 183 and A. niger MTCC 282 strains were purchased from MTCC, Chandigarh, India. Chemical reactions were monitored by TLC on silica gel plates in iodine and UV chambers. Sonar melting point apparatus in open capillary tube was used for the recording of melting points. ¹H NMR and ¹³C NMR spectra were confirmed in DMSO and deuterated CDCl₃ on Bruker Avance II 400 NMR spectrometer at a frequency of 400 MHz downfield to tetramethyl silane standard. FTIR spectra were recorded on Perkin Elmer FTIR spectrophotometer with the help of KBr pellets technique. Waters Micromass Q-ToF Micro instrument was used for Mass spectrum recording.

All the reactions were performed in oven-dried glassware. All reagents and solvents were used as obtained from the supplier or recrystallized/redistilled unless otherwise noted. The purity of the synthesized compounds was monitored by ascending thin layer chromatography (TLC) on silica gel-G (Merck, Darmstadt, Germany) coated aluminum plates, visualized by iodine vapor. Melting points were determined in open capillary tubes and are uncorrected. Infrared (IR) spectra were recorded on a PS 4000 FTIR instrument (JASCO, Tokyo, Japan) using KBr pellets. Elemental analyses (C, H, and N) were done with a FLASHEA 112 analyzer (Shimadzu, Mumbai, Maharashtra, India) and all analyses were consistent (within 0.4%) with theoretical values. The ¹H-NMR and ¹³C-NMR spectra of synthesized compounds were recorded on an Avance II 400 NMR spectrometer (Bruker, Billerica, MA, USA) at 400/100 MHz frequency in DMSO-d₆ or CDCl₃ and using TMS as internal standard (chemical shift δ values are expressed in ppm). Mass spectra were scanned on a Micromass Q-Tof system (Waters, Manchester, UK) [26 (link)].

All the reactions were performed in oven-dried glasswares. All reagents and solvents were used as obtained from the supplier or recrystallized/redistilled unless otherwise noted. The ultrasound sonicator (Sonics Vibra-cell, Modelno. VCX 500, Newtown, CT, USA) equipped with solid synthetic probe, 13 mm in tip diameter, operating at 20 kHz with a maximum power output of 500 W, was used for synthesis of final title compounds. The purity of the synthesized compounds was monitored by ascending thin layer chromatography (TLC) on silica gel-G (Merck, Darmstadt, Germany) coated aluminum plates, visualized by iodine vapor and melting points were determined in open capillary tubes. Infrared (IR) spectra were recorded on a PS 4000 FTIR (JASCO, Tokyo, Japan) using KBr pellets. Elemental analyses (C, H, and N) were done with a FLASHEA 112 Shimadzu’ analyzer (Mumbai, Maharashtra, India) and all analyses were consistent (within 0.4%) with theoretical values. The ¹H-NMR and ¹³C-NMR spectra of synthesized compounds were recorded on Bruker Avance II 400 NMR Spectrometer (Billerica, MA, USA) at 400 MHz Frequency in deuterated DMSO and CDCl₃ and using TMS as internal standard (chemical shift δ in ppm). Mass spectra of some compounds were scanned on FTMS + p ESI full mass (100.00–1500.00).

Unless otherwise noted, the chemicals required for synthesis and antioxidant activity were purchased from Hi-media Laboratories. The biological hMAO activity evaluation of the test drugs was examined by quantifying their action on the generation of H₂O₂ by p-tyramine (general substrate for hMAO-B and hMAO-A), utilizing the Amplex Red MAO assay kit (Sigma USA) and MAO isoforms (microsomal) obtained from insect cells (BTI-TN-5B14) expressed as recombinant baculovirus consisting cDNA probes for hMAO-A or hMAO-B. Reactions were monitored by thin layer chromatography TLC executed over silica gel precoated plates (0.25 mm) purchased from Merck, envisioned of single spots was carried in iodine and UV chambers, in mobile media TLC- Benzene:Chloroform (7:3). Melting points were recorded on Sonar melting point apparatus in open capillary tubes. The nuclear magnetic resonance (NMR) spectra ¹H NMR and ¹³C NMR spectra were confirmed in DMSO and deuterated CDCl₃ respectively on Bruker Avance II 400 NMR spectrometer at a frequency of 400 MHz downfield to tetramethylsilane standard. Coupling constants (J) were reported in Hertz (Hz) and chemical shifts were depicted as d (parts per million). Infrared (IR) spectra were recorded on Perkin Elmer FTIR spectrophotometer by using KBr pellets technique. Waters Micromass Q-ToF Micro instrument was used for Mass spectra recording.

The chemical structure of carrageenans isolated from the red alga Chondrus armatus, as well as their low molecular weight derivatives, was confirmed by Infrared spectroscopy. IR spectra were recorded on an IR Affinity-1S spectrometer (Shimadzu, Japan) using an attenuated total internal reflection attachment. The determination was carried out under the following conditions: spectral range in the range of 2000–600 cm⁻¹, resolution 4 cm⁻¹, number of scans 64. The LabSolutions IR 2.13 software (Shimadzu, Tokyo, Japan) was used to analyze the spectra (Figure 1B).
An NMR spectrum was obtained using an Avance II 400 NMR spectrometer (Bruker, Berlin, Germany) resonating at 100 MHz at 70 °C. The concentration of the samples was 5–7 mg of polysaccharide/mL of D₂O. The 13C NMR analysis was performed in 36,000 scans.
The molecular weight distribution was determined by high performance size exclusion chromatography on a Shimadzu LC-20AD chromatograph equipped with a Shodex OHpak SB-804MHQ analytical column (Shimadzu, Kyoto, Japan). A 0.1 M NaNO₃ solution was used as the mobile phase with a flow rate of 0.8 mL/min. To determine the molecular weights of the analyzed samples of carrageenans, they were built according to standard samples of pullulans (Figure 2b).