UV spectra were recorded on a PerkinElmer Lambda spectrophotometer. The NMR experiments were performed on a Bruker DRX-600 spectrometer at 300 K. The mass spectrometry analyses were performed with a Q-TOF premier spectrometer (Waters, Milford, MA, USA), coupled with an Alliance HPLC module (Waters, Milford, MA, USA). TLC was performed on precoated Kieselgel 60 F254 plates (Merck, Darmstadt, Germany). Column chromatography was performed over Sephadex LH-20 (Pharmacia); reversed-phase (RP) HPLC separations were conducted on a Shimadzu LC-8A series pumping system equipped with a Shimadzu RID10 A refractive index detector and a Shimadzu injector, using a Bondapak C18 column (30 cm × 7.8 mm, 10 µm, Waters, Milford, MA, USA). A Metrohm 827 pH meter, a two-channel laboratory pH measuring instrument for measuring pH/mV and temperature, was used for the pH measurement. The UE was carried out using a 320 W Ultrasonic bath (Branson 2510E-MTH, Bransonic®). The sample was placed in an Erlenmayer flask with the corresponding amount of solvent and was treated with ultrasound at 25°C for a given duration (Table 1 ). MAE was performed using a multimodal household microwave oven Silvercrest SMW 700 A1 at 700 W and a 100 mL flask exposed to microwave irradiation (irradiation cycle: 10 s power on, followed by 10 s power off) for a given duration (Table 1 ) [13 (link)–15 ].
Q tof premier spectrometer
Manufactured by Waters Corporation
Sourced in United States
The Q-TOF Premier spectrometer is a high-performance mass spectrometry instrument designed for accurate mass measurements and structural characterization of a wide range of analytes. It combines a quadrupole mass analyzer with a time-of-flight (TOF) mass analyzer, providing high resolution and sensitivity.
Automatically generated - may contain errors
Lab products found in correlation
Rid 10a refractive index detector, by Shimadzu (3 mentions)
Drx 600 spectrometer, by Bruker (3 mentions)
Kieselgel 60 f254 plate, by Merck Group (3 mentions)
Lc 8a series pumping system, by Shimadzu (2 mentions)
Bondapak c18 column, by Waters Corporation (1 mentions)
2510e mth, by Emerson (1 mentions)
Avance spectrometer, by Bruker (1 mentions)
Avance 3 400 spectrometer, by Bruker (1 mentions)
Toyopearl gel hw 40f, by Tosoh (1 mentions)
1525 hplc, by Waters Corporation (1 mentions)
Sephadex lh 20, by Cytiva (1 mentions)
C18 μ bondapak column, by Waters Corporation (1 mentions)
241 polarimeter, by PerkinElmer (1 mentions)
Ce so4 2 h2so4, by Merck Group (1 mentions)
Methanol d4, by Merck Group (1 mentions)
Autopol 4 polarimeter, by Rudolph Research Analytical (1 mentions)
Lc 20at series pumping system, by Shimadzu (1 mentions)
Silica gel, by Merck Group (1 mentions)
5 mm tci cryoprobe, by Bruker (1 mentions)
P 1020 polarimeter, by Jasco (1 mentions)
10 protocols using q tof premier spectrometer
1
Analytical Techniques for Natural Product Characterization
2
Purification and Characterization of Organic Compounds
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Unless otherwise specified, the reagents were purchased from commercial suppliers and used without further purification. All reactions were conducted under N2 atmosphere using undistilled solvent. Analytical thin layer chromatography (TLC) was performed using silica gel plate (0.2 mm thickness). Subsequent to elution, plates were visualized using UV radiation (254 nm). Flash chromatography was performed using Merck silica gel (200–300 mesh) for column chromatography with freshly distilled solvents. IR spectra were recorded on an FT-IR spectrophotometer using KBr optics. 1H and 13C NMR spectra were recorded in CDCl3 and DMSO-d6 on Bruker Avance or Jeol 400 MHz spectrometers. The chemical shifts (δ) are reported in ppm and coupling constants (J) in Hz. NMR splitting patterns are designated as singlet (s), doublet (d), triplet (t), quartet (q), multiplet (m), doublet of doublets (dd), doublet of triplets (dt), doublet of quartets (dq), triplet of doublets (td), triplet of triplets (tt), quartet of doublets (qd), doublet of doublet of doublets (ddd), etc. Tetramethylsilane (TMS) served as internal standard for 1H and 13C NMR analysis. High resolution mass spectra (HRMS) were obtained via a Waters Q-TOF Premier Spectrometer (ESI source).
3
Synthesis and Characterization of Novel Organic Compounds
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All solvents and reagents were commercially available, and were used without further purification unless stated. The progress of the reactions was monitored by thin-layer chromatography on a glass plate coated with silica gel with a fluorescent indicator (GF254, Qingdao Ocean Chemicals, China). The melting point of target compounds were detected on the RD-1 melting apparatus (Tianjin Guoming Medical Equipment Co., LTD, China). The 1 H and 13 C nuclear magnetic resonance (NMR) spectra were recorded on a model 600 Bruker Avance spectrometer (Bruker, Germany) at 600 and 150 MHz, respectively. Chemical shifts are given in parts per million (δ) referenced to DMSO-d6 at δ 2.50 for 1 H and δ 39.5 for 13 C. High-resolution mass spectra (HRMS) of target compounds were performed by a Waters Q-TOF Premier spectrometer (Waters, USA).
4
Analytical Techniques for Natural Product Characterization
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NMR spectra were recorded on Bruker AVANCE III-400 spectrometer using CDCl3 and CD3OD as solvents. Chemical shifts were reported in parts per million (ppm, δ) downfield from tetramethylsilane. HR-TOF-MS were determined by a quadruple time of flight (Q-TOF) premier spectrometer coupled with an ESI source (Waters Co., Ltd, Milford, USA). Column chromatography procedures were performed using silica gel (200–400 mesh, Qingdao Marine Chemical Ltd., China), MCI resin CHP 20P (Mitsubishi Chemistry Co. Ltd., Japan), Toyopearl gel HW-40F (TOSOH Co., Ltd., Japan), and Sephadex LH-20 (25–100 μm, Pharmacia Fine Chemical Industries Co. Ltd., Sweden). Thin-layer chromatography (TLC) was performed using silica gel GF254 precoated plates (Qingdao Marine Chemical Ltd., China). After spraying with a color reagent (10% vanillin-H2SO4 and 10% H2SO4 in EtOH), heating revealed the spots. All reagents were purchased from commercial sources without further purification.
5
Synthesis and Characterization of PACAP 1-38
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The peptide PACAP 1–38 was synthesized on a Liberty Blue peptide synthesizer (CEM Corp.) as a C-terminal amide at 0.025 mM scale using standard Fmoc synthetic methods and piperidine deprotection. The peptide was cleaved from resin and deprotected using a trifluoroacetic acid cocktail at 37°C for 30 min and precipitated using ice-cold diethyl ether. The crude peptide was purified on a Waters 1525 HPLC and Sunfire semi-prep C18 column, fitted with a 2998 photodiode array detector, using a linear gradient of water/acetonitrile, each containing 0.2% trifluoroacetic acid. Fractions containing the peptide were combined and lyophilized overnight. The fluffy white residue was analyzed by a Waters QToF Premier spectrometer in positive ion mode. Strong peaks for M +3, +4, +5 … +8 were observed, for a deconvoluted mass of 4515 Da (calculated mass 4534 Da), indicating a loss of water in the spectrometer. The HPLC trace at 220 nm absorbance indicates two peaks at 10.9 and 14.6 min which may indicate the folded and unfolded forms of the peptide.
6
Analytical Methods for Compound Characterization
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Briefly optical rotations were measured on a Perkin-Elmer 241 polarimeter equipped with a sodium lamp (589 nm) and a 1 dm microcell. UV spectra were recorded on a Perkin-Elmer-Lambda spectrophotometer. NMR experiments were performed on a Bruker DRX-600 spectrometer at 300 K. HRESIMS were acquired in positive ion mode on a Q-TOF premier spectrometer equipped with a nanoelectrospray ion source (Waters-Milford, MA, USA). Column chromatography was performed over Sephadex LH-20 (Amersham Biosciences; Uppsala, Sweden). Silica gel 60 (0.040–0.063 mm; Carlo Erba; Milan, Italy) was used as column material. HPLC separation was conducted on a Shimadzu LC-8A series pumping system equipped with a Shimadzu RID-10A refractive index detector and Shimadzu injector on a C18μ-Bondapak column (30 cm x 7.8 mm, 10 μm Waters, flow rate 2.0 mL min−1). TLC was performed on precoated Kiesel gel 60 F254 plates (Merck; Darmstadt, Germany); compounds were detected by Ce(SO4)2/H2SO4 (Sigma-Aldrich, Milan, Italy) solution; and reagent grade chemicals (Carlo Erba; Milan, Italy) were used throughout [6 (link), 7 (link)].
7
Structural Characterization of Natural Compounds
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Optical rotations were measured on a Rudolph Research Analytical Autopol IV polarimeter equipped with a sodium lamp (589 nm) and a 1-dm microcell. NMR experiments were performed on a Bruker DRX-600 spectrometer (Bruker BioSpin GmBH, Rheinstetten, Germany) equipped with a Bruker 5-mm TCI CryoProbe at 300 K. All 2D NMR spectra were acquired in methanol-d4 (99.95%, Sigma-Aldrich, St. Louis, MO, USA), and standard pulse sequences and phase cycling were used for DQF-COSY, HSQC, and HMBC spectra. ESI-MS were obtained using a Finnigan LC-Q Advantage Thermoquest spectrometer, equipped with Xcalibur software. HR-ESIMS spectra were acquired in positive ion mode on a Q-TOF premier spectrometer (Waters, Milford, Massachusetts, USA). TLC was performed on pre-coated Kieselgel 60 F254 plates (Merck KGaA, Darmstadt, Germany); compounds were detected by spraying with Ce(SO4)2/H2SO4 solution. Column chromatography was performed over silica gel (70–220 mesh, Merck); reversed-phase (RP) HPLC separations were conducted on a Shimadzu LC-20AT series pumping system equipped with a Shimadzu RID10A refractive index detector and a Shimadzu injector.
8
Synthesis and Characterization of Aryl Fluorosulfates and Formates
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Unless otherwise stated, all reagents were purchased from commercial suppliers and used without further purification. All the aryl fluorosulfates 1 and aryl formates 2 were prepared by following reported method [40 (link),73 (link),80 (link)]. Analytical thin layer chromatography (TLC) was performed using silica gel plate (0.2 mm thickness). Subsequent to elution, plates were visualized using UV radiation (254 nm). Flash chromatography was performed using Merck silica gel (200–300 mesh) for column chromatography with freshly distilled solvents. IR spectra were recorded on a FT-IR spectrophotometer using KBr optics. 1H, 13C, and 19F NMR spectra were recorded in CDCl3 on Bruker Avance or Jeol 400 MHz spectrometers. Tetramethylsilane (TMS) served as internal standard for 1H, 13C and 19F NMR analysis. High resolution mass spectra (HRMS) were obtained on a Waters Q-TOF Premier Spectrometer (ESI source).
9
Spectroscopic Characterization of Compounds
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Optical rotation was measured using a Jasco P-1020 polarimeter (Jasco, Tokyo, Japan). Nuclear magnetic resonance (NMR) spectra were recorded on a Bruker (AM 500 MHz) FT-NMR spectrometer using tetramethylsilane as an internal standard. High-resolution electrospray ionization mass spectrometry (HRESIMS) was performed using a Waters Q-TOF Premier spectrometer. All solvents used for column chromatography were of analytical grade (SK Chemicals Co., Ltd., Seongnam-si, Korea). The solvents used for ultra-performance liquid chromatography (UPLC) were of liquid chromatography/mass spectrometry (LC/MS) grade (SK Chemicals Co., Ltd.).
10
Synthesis and Characterization of Organic Compounds
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