The structure of isolated compound was determined by different spectroscopic analyses such as IR, NMR spectra (1H NMR, 13C DEPT 135 and DEPT 90), and two-dimensional experiments, such as hydrogen–hydrogen correlation (H–H COSY), heteronuclear multiple bond coherence (HMBC), heteronuclear single quantum coherence (HSQC), mass spectrometry, and also by comparison with literature data. For obtaining IR spectrum, we used a Bruker Tensor 27 spectrometer coupled with ATR. 1H NMR and 13C NMR were acquired on a Bruker Avance III, operating in 400 MHz for 1H NMR and 100 MHz for 13C NMR. Samples were dissolved in CD3 OD. Chemical shifts were given in δ (ppm), and coupling constants (J) are expressed in Hertz (Hz). Residual not deuterated solvent peak (δH 4.87, 3.31 and δC 49.15) was set as reference, and tetramethylsilane (TMS) was used as an internal standard. DART-MS (Direct Analysis in Real Time Mass Spectrometry) was measured using a Joel AccuTOF JMS-T100 LC Mass Spectrometer (Japan) and positive ion [M+ H+] was identified. Fourier-transform infrared (FT-IR) spectra were taken on a Bruker Tensor 27 spectrometer with photodiode detector using KBr pellets method for sample preparation.
Tensor 27 spectrometer
Manufactured by Bruker
Sourced in Germany, United States, United Kingdom, Japan, Switzerland
The Tensor 27 is a Fourier Transform Infrared (FTIR) spectrometer manufactured by Bruker. It is designed for routine analysis and research applications in various fields such as chemistry, materials science, and life sciences. The Tensor 27 provides high-quality infrared spectroscopy data and enables users to identify and characterize a wide range of organic and inorganic compounds.
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Lab products found in correlation
Drx 300 avance instrument, by Bruker (13 mentions)
Opus software, by Bruker (10 mentions)
5975c vl msd, by Agilent Technologies (10 mentions)
Silica gel, by Qingdao Haiyang Chemical (9 mentions)
Opus 8, by Bruker (9 mentions)
Znse atr element, by Bruker (6 mentions)
D8 advance, by Bruker (5 mentions)
Bioatr 2, by Bruker (5 mentions)
P 1020 polarimeter, by Jasco (4 mentions)
Av 600 mhz spectrometer, by Bruker (4 mentions)
Microtof spectrometer, by Bruker (4 mentions)
Smart apex 2 ccd diffractometer, by Bruker (4 mentions)
Dd2400 mhz spectrometer, by Bruker (4 mentions)
S 4800, by Hitachi (4 mentions)
Zetasizer nano zs90, by Malvern Panalytical (3 mentions)
Autosystem xl, by PerkinElmer (3 mentions)
Uv 2450 spectrophotometer, by Shimadzu (3 mentions)
Hts xt, by Bruker (3 mentions)
Spectramax 190, by Molecular Devices (3 mentions)
Fv1000 confocal microscopy, by Olympus (3 mentions)
322 protocols using tensor 27 spectrometer
1
Spectroscopic Characterization of Isolated Compound
2
ATR-FTIR Spectroscopy of Immobilized Biomolecules
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Appropriate IB samples were placed and dried with a continuous N2 flow, on spectroscopic crystal surfaces. Total reflectance spectroscopy was determined 16 times in form of spectra. A scan rate of 50 cm−1/min with a nominal resolution of 2 cm−1 was used, in a Tensor 27 Bruker spectrometer with a Specac’s Golden Gate Attenuated Total Reflectance (ATR) accessory. Measurements were always conducted at 25 °C under a stream of N2. The absorbance values were corrected by subtracting the background. Fourier deconvolution of the spectra and the second derivative allowed the identification and analyses of different band components. According to the previously described procedure, fitting the components to the original (not deconvolved) spectrum was performed [53 (link)], assuming a Gaussian shape. Data were treated by using the Peakfit software.
3
Characterization of Micellar Nanoparticles for Drug Delivery
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1H NMR spectra were obtained using a Bruker Avance 400 MHz instrument (Switzerland). CDCl3 was used as the solvent. The mean particle size and ζ-potential of micellar aggregates were determined by dynamic light scattering (DLS) using a Malvern Zetasizer Nano ZS90 (Malvern, UK). DLS samples (micelles with/without DOX-loaded) were prepared in water, and was filtered using a 0.22 μm Nylon Syringe Filter prior to the measurements. The molecular weight distribution was determined by gel permeation chromatography (GPC) equipped with a 1260 Infinity Isocratic Pump and an RI detector (Agilent, US). DMF containing 0.1 mol% LiBr was the elute and the flow rate was 1.0 mL/min. Linear poly(methyl methacrylate) standards from Fluka were used for calibration. FT-IR spectra were recorded in ATR mode (Golden gate) on a Tensor 27 Bruker spectrometer (Germany). The particles were imaged using a Tecnai G2 F20 TWIN transmission electron microscope operated at 200 kV and equipped with a field-emission gun (FEI, Netherland). The sample was placed onto a Quantifoil grid, followed by utilizing Vitrobot, and then flash frozen in liquid ethane. The images were recorded at magnification of 14,500 and 25,000 with a 4 K * 4 K eagle CCD camera and defocus ranging from 2 to 3 μm. Confocal images of the samples were taken using the Leica TCS SP5 (Germany).
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1H NMR spectra were obtained using a Bruker Avance 400 MHz instrument (Switzerland). CDCl3 was used as the solvent. The mean particle size and ζ-potential of micellar aggregates were determined by dynamic light scattering (DLS) using a Malvern Zetasizer Nano ZS90 (Malvern, UK). DLS samples (micelles with/without DOX-loaded) were prepared in water, and was filtered using a 0.22 μm Nylon Syringe Filter prior to the measurements. The molecular weight distribution was determined by gel permeation chromatography (GPC) equipped with a 1260 Infinity Isocratic Pump and an RI detector (Agilent, US). DMF containing 0.1 mol% LiBr was the elute and the flow rate was 1.0 mL/min. Linear poly(methyl methacrylate) standards from Fluka were used for calibration. FT-IR spectra were recorded in ATR mode (Golden gate) on a Tensor 27 Bruker spectrometer (Germany). The particles were imaged using a Tecnai G2 F20 TWIN transmission electron microscope operated at 200 kV and equipped with a field-emission gun (FEI, Netherland). The sample was placed onto a Quantifoil grid, followed by utilizing Vitrobot, and then flash frozen in liquid ethane. The images were recorded at magnification of 14,500 and 25,000 with a 4 K * 4 K eagle CCD camera and defocus ranging from 2 to 3 μm. Confocal images of the samples were taken using the Leica TCS SP5 (Germany).
4
Multimodal Characterization of Polymers
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1H NMR spectra were recorded on 1.5% wt. solutions in deuterated chloroform and dimethyl sulfoxide (d6-DMSO) using a Bruker Avance 300 or 400 MHz Bruker spectrometer.
FT-IR spectra were recorded in ATR mode (Golden Gate) on a Tensor 27 Bruker spectrometer (Bruker UK Limited, UK) equipped with a 3000 Series TM High Stability Temperature Controller (Specac, UK).
Gel permeation chromatography (GPC) analysis was performed using triple detection conditions with a Malvern OmniSec System (Malvern, UK) comprising of a D6000M and D3000 column in sequence and operating online at 50 °C with HPLC grade DMF containing 0.1% LiBr as the mobile phase at a flow rate of 1.0 mL/min. Calibration was performed using a poly(methyl methacrylate) standard of a known molecular weight, intrinsic viscosity, and dn/dc.
UV-Vis and fluorescence readings were obtained through a BioTek Synergy 2 multimode microplate reader (BioTek, UK) at a temperature of 37 °C.
FT-IR spectra were recorded in ATR mode (Golden Gate) on a Tensor 27 Bruker spectrometer (Bruker UK Limited, UK) equipped with a 3000 Series TM High Stability Temperature Controller (Specac, UK).
Gel permeation chromatography (GPC) analysis was performed using triple detection conditions with a Malvern OmniSec System (Malvern, UK) comprising of a D6000M and D3000 column in sequence and operating online at 50 °C with HPLC grade DMF containing 0.1% LiBr as the mobile phase at a flow rate of 1.0 mL/min. Calibration was performed using a poly(methyl methacrylate) standard of a known molecular weight, intrinsic viscosity, and dn/dc.
UV-Vis and fluorescence readings were obtained through a BioTek Synergy 2 multimode microplate reader (BioTek, UK) at a temperature of 37 °C.
5
Synthesis and Characterization of n-12-n(OH) Derivative
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Ethyl isocyanate (0.32 mL, 4 mM) was added to a stirred solution of n-12-n(OH) (1 mM) and DABCO (0.05 g). The reaction mixture was stirred for 16 h at 333 K in 30 mL dry acetonitrile. The solvent was removed under vacuum (20 mm Hg), and the product was recrystallized from ethyl acetate/acetone. The precipitate was filtered and dried on a water bath (313 K) under vacuum (15 mm Hg). Data from elemental analysis, IR spectroscopy, 1H NMR spectroscopy, and mass spectrometry were used to confirm the structures of the compounds. 1H NMR spectra were recorded on a Bruker Avance NMR 1H spectrometer. Mass spectra with electrospray ionization (ESI) were obtained on a Bruker AmaZon X Ion Trap mass-spectrometer (Bruker GmbH, Mannheim, Germany), and the results were processed using DataAnalysis 4.0 SP4 software. Elemental analysis was carried out on a EuroEA3028-HT-OM CHNS analyzer (Eurovector SpA, Pavia, Italy), and the results were processed using Callidus 4.1 software. IR spectra were recorded on a Tensor 27 Bruker spectrometer (Bruker GmbH, Mannheim, Germany) in KBr pellets, and the results were processed using OPUS 7/2012 software.
6
ATR Spectroscopy with Thermal Control
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Spectra were recorded in ATR mode
(Golden Gate) on a Tensor 27 Bruker spectrometer (Bruker UK Limited,
UK) equipped with a 3000 Series TM High Stability Temperature Controller
with RS232 Control (Specac, UK).
(Golden Gate) on a Tensor 27 Bruker spectrometer (Bruker UK Limited,
UK) equipped with a 3000 Series TM High Stability Temperature Controller
with RS232 Control (Specac, UK).
7
FTIR Analysis of Powder Composition
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The chemical composition of the powders was analyzed using Fourier Transform Infrared Spectroscopy (FTIR; Bruker Tensor 27 spectrometer; Bruker Corporation, Billerica, MA, USA). FTIR spectra were recorded in Attenuated Total Reflectance (ATR) mode. Spectra were obtained at a resolution of 4 cm−1, over a range of wavenumbers from 400 cm−1 to 4000 cm−1, with an average of 50 scans. Before every measurement, a background spectrum was taken and deducted from the sample spectrum.
8
Synthesis and Characterization of Novel Compounds
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All chemicals (reagent grade) used were purchased from Sino Pharm Chemical Reagent Co., Ltd. (Shanghai, China). Reaction progress was monitored using analytical thin layer chromatography (TLC) on precoated silica gel GF254 (Qingdao Haiyang Chemical Plant, Qing-Dao, China) plates and the spots were detected under UV light (254 nm). Melting point was measured on an XT-4 micromelting point instrument and uncorrected. IR (KBr-disc) spectra were recorded by Bruker Tensor 27 spectrometer (Billerica, MA).
1H NMR and 13C NMR spectra were measured on a BRUKER AVANCE III spectrometer (Billerica, MA) at 25 °C and referenced to TMS. Chemical shifts are reported in ppm (δ) using the residual solvent line as internal standard. Splitting patterns are designed as s, singlet; d, doublet; t, triplet; m, multiplet. The purity of all compounds was confirmed to be higher than 95% through analytical HPLC performed with Agilent 1200 HPLC System (Santa Clara, CA). Mass spectra were obtained on a MS Agilent 1100 Series LC/MSD Trap mass spectrometer (ESI-MS) (Santa Clara, CA).
1H NMR and 13C NMR spectra were measured on a BRUKER AVANCE III spectrometer (Billerica, MA) at 25 °C and referenced to TMS. Chemical shifts are reported in ppm (δ) using the residual solvent line as internal standard. Splitting patterns are designed as s, singlet; d, doublet; t, triplet; m, multiplet. The purity of all compounds was confirmed to be higher than 95% through analytical HPLC performed with Agilent 1200 HPLC System (Santa Clara, CA). Mass spectra were obtained on a MS Agilent 1100 Series LC/MSD Trap mass spectrometer (ESI-MS) (Santa Clara, CA).
9
Analytical Techniques for Natural Product Isolation and Characterization
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Silica gel (200–300 and 400–600 mesh, Qingdao Marine Chemical Co., Qingdao, China) and Sephadex LH–20 (Pharmacia Co., Stockholm, Sweden) were used for column chromatography (CC) and thin-layer chromatography (TLC). Analytical HPLC was performed on a Surveyor high performance liquid chromatography system (Thermo Fisher Co., Waltham, MA, USA) with an Alltech 2000ES evaporative light scattering detector (Alltech Co., Nicholasville, KY, USA). Preparative HPLC (Rp–C18: 21.2 × 150 mm, 5 μm, Innoval C18, Agela Technologies Co. Ltd., Tianjin, China) was carried out on a KNAUER apparatus with a refractive index detector (Knauer Co., Berlin, Germany). IR data were recorded on a Bruker Tensor–27 spectrometer (Bruker Co., Billerica, MA, USA). High–resolution electrospray ionization mass spectrometry (HR-ESI-MS) was performed on the Agilent G6230A TOF LC/MS (Agilent Technologies Co. Ltd., Santa Clara, CA, USA). Both 1D and 2D NMR spectra were recorded on a Bruker ECA–400 MHz spectrometer (Bruker Co., Billerica, MA, USA) with TMS as an internal standard, and chemical shifts are expressed in d (ppm). ECD spectra were recorded in methanol using a JASCO J–815 spectrophotometer (Jasco International Co., Ltd., Tokyo, Japan) at room temperature.
10
Physicochemical Characterization of Purified Compounds
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The purification process was controlled by gas chromatography (Autosystem XL) (PerkinElmer, Waltham, MA, USA) coupled with a flame ionization detector (FID) (PerkinElmer, Waltham, MA, USA) and an HP-5 (30 m × 0.25 mm × 0.25 μm) capillary column (Agilent Technologies, Santa Clara, CA, USA). In the investigations, the TurboChrom 6.1 software (PerkinElmer, Waltham, MA, USA), was used.
The following apparatus was used to evaluate the physicochemical properties: Bruker Tensor 27 spectrometer (Bruker, Billerica, MA, USA) with an ATR accessory and OPUS software (Bruker); BROOKFIELD LVDV-II + viscometer (Labo-Plus, Warsaw, Poland); DMA 4500 M (Anton Paar, Graz, Austria).
The following apparatus was used to evaluate the physicochemical properties: Bruker Tensor 27 spectrometer (Bruker, Billerica, MA, USA) with an ATR accessory and OPUS software (Bruker); BROOKFIELD LVDV-II + viscometer (Labo-Plus, Warsaw, Poland); DMA 4500 M (Anton Paar, Graz, Austria).
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