All reactions were performed, excluding moisture, dried solvents, and uncorrected melting points. The IR spectra were recorded as potassium bromide pallets on an Aldrich FT-IR spectrometer (Central Laboratory at Faculty of Science, Benha, Ain Shams, and Cairo Universities). Mass spectra were recorded on GCMS (gas chromatography–mass spectrometer) Shimadzu QP- 2010 Plus (Microanalytical center, Ain shams University). Elemental analysis was determined using UV light on the Ain Shams University elementary analysis system. The Bruker Spectro spin DPX-400MHz was used to record the 1H NMR (500 MHz, DMSO-d6) and 13C NMR (125 MHz, Chloroform-d) spectra. Chemical shift (d) values were stated in parts per million (ppm) using internal standard tetramethylsilane. The D2O exchange confirmed that the exchangeable protons (OH and NH) and some other labial hydrogens are exchangeable. LC–MS/MS (PerkinElmer) was used to record the mass spectra, presented as m/z. Elemental analysis was achieved using the PerkinElmer 240 analyzer. The purity of synthesized compounds and the progress of the reaction were evaluated by ascending thin layer chromatography (TLC) (silica gel Fluka, 706, 43-50 EA) using methanol/chloroform (9:1 v/v) and methylene chloride/chloroform (4:1 v/v) as a solvent system.
Qp2010 plus
Manufactured by Shimadzu
Sourced in Japan, United States, United Kingdom
The QP2010 Plus is a Gas Chromatograph-Mass Spectrometer (GC-MS) system manufactured by Shimadzu. It is designed to perform qualitative and quantitative analysis of complex samples by combining the separation capabilities of gas chromatography with the identification and detection capabilities of mass spectrometry.
Automatically generated - may contain errors
Lab products found in correlation
Gcms2010 plus, by Shimadzu (3 mentions)
Gc 2010, by Shimadzu (3 mentions)
Software gc ms solution v 2, by Shimadzu (3 mentions)
Qp 2010 system, by Shimadzu (3 mentions)
Rtx 5ms, by Restek (3 mentions)
Gc ms, by Shimadzu (3 mentions)
Ft ir spectrometer, by Merck Group (2 mentions)
Gcms solution v 4.45sp1, by Shimadzu (2 mentions)
Db wax column, by Agilent Technologies (2 mentions)
Rtx wax column, by Restek (2 mentions)
Turbomatrix 300 td, by PerkinElmer (2 mentions)
Rtx 5ms column, by Shimadzu (2 mentions)
Qp2020, by Shimadzu (2 mentions)
N alkanes c8 c40, by Merck Group (2 mentions)
Spectrospin dpx 400mhz, by Bruker (1 mentions)
Ir 435 spectrophotometer, by Shimadzu (1 mentions)
Gemini 300 bb spectrophotometer, by Bruker (1 mentions)
Silica gel g, by Merck Group (1 mentions)
Ultimate 3000 lc system, by Thermo Fisher Scientific (1 mentions)
Q exactive, by Thermo Fisher Scientific (1 mentions)
123 protocols using qp2010 plus
1
Comprehensive Spectroscopic Characterization of Synthesized Compounds
2
Melting Point and Spectroscopic Analysis of Organic Compounds
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Melting points were uncorrected and determined on a Stuart melting point apparatus (Stuart Scientific, Redhill, UK). Elemental analyses of C, H and N were performed on a Perkin-Elmer 2400 analyzer (Perkin-Elmer, Norwalk, CT, USA). The IR spectra (KBr) were measured on a Shimadzu IR 435 spectrophotometer and the values are represented in cm−1. 1H NMR (400 MHz) and 13C NMR (75 MHz) spectra were carried out using a Varian Gemini 300-BB spectrophotometer (Bruker, Munich, Germany). Splitting patterns were designated as follows: s: singlet; d: doublet; t: triplet; m: multiplet, and chemical shift values were recorded in ppm on a scale. Mass spectra were run on a Shimadzu Qp-2010 plus. The progress of the reactions was monitored by TLC using TLC sheets pre-coated with UV florescent silica gel (Merck 60 F 254), and was visualized using a UV lamp. The chemicals used were supplied from Acros (New Jersey, USA).
3
Comprehensive Analytical Characterization
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Melting points
were determined on a MEL-TEMP II melting point apparatus in open glass
capillaries. The homogeneity of the products and follow up of the
reactions were checked by thin layer chromatography (TLC) on plates
precoated with silica gel G (Merck; layer thickness 0.25 mm), used
without pretreatment. All ratios of the used solvent systems were
volume to volume (V/V); the distance of the solvent travel was 5 cm,
and the spots were visualized by exposure to iodine vapor for a few
minutes. The infrared spectra (IR) were recorded for potassium bromide
(KBr) discs on a PerkinElmer USA spectrophotometer, model 1430, covering
the frequency range of 200–4000 cm–1. Proton
magnetic resonance (1H NMR) spectra were carried out at
ambient temperature (∼25 °C) with Joule JNM ECA 500 MHz
or with Bruker 400 MHz spectrometers using tetramethylsilane (TMS)
as an internal standard; the chemical shifts are reported in parts
per million on the δ scale. Mass spectra (MS) were performed
on a GCMS solution DI Analysis Shimadzu Qp-2010 Plus. Elemental microanalyses
were performed at the Microanalytical Unit, Cairo University, Cairo,
Egypt. Antimicrobial activity of the screened samples was carried
out at the Faculty of Pharmacy, Pharmaceutical Microbiology Lab, Alexandria
University.
were determined on a MEL-TEMP II melting point apparatus in open glass
capillaries. The homogeneity of the products and follow up of the
reactions were checked by thin layer chromatography (TLC) on plates
precoated with silica gel G (Merck; layer thickness 0.25 mm), used
without pretreatment. All ratios of the used solvent systems were
volume to volume (V/V); the distance of the solvent travel was 5 cm,
and the spots were visualized by exposure to iodine vapor for a few
minutes. The infrared spectra (IR) were recorded for potassium bromide
(KBr) discs on a PerkinElmer USA spectrophotometer, model 1430, covering
the frequency range of 200–4000 cm–1. Proton
magnetic resonance (1H NMR) spectra were carried out at
ambient temperature (∼25 °C) with Joule JNM ECA 500 MHz
or with Bruker 400 MHz spectrometers using tetramethylsilane (TMS)
as an internal standard; the chemical shifts are reported in parts
per million on the δ scale. Mass spectra (MS) were performed
on a GCMS solution DI Analysis Shimadzu Qp-2010 Plus. Elemental microanalyses
were performed at the Microanalytical Unit, Cairo University, Cairo,
Egypt. Antimicrobial activity of the screened samples was carried
out at the Faculty of Pharmacy, Pharmaceutical Microbiology Lab, Alexandria
University.
4
Blueberry Volatile Compounds Analysis
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Blueberry VOCs were analyzed by gas chromatography coupled with mass spectrometry (GC-MS) using a Shimadzu QP 2010 PLUS (Shimadzu Corp., Tokyo, Japan) equipped with a Rtx®-5MS column (30 m, 0.25 mm i.d, 0.25 mm lm thickness; Alltech, USA). Samples (1 μl) were injected in the splitless mode with He as carrier gas at a ow rate of 1 ml/min (49.7 KPa). The oven temperature was programmed from 40 °C for 4 min, then increased to 150 °C at 5°C/min and to 250 °C at 10°C/min (held for 10 min). Injector and MS transfer line temperatures were both set at 250 °C.
Volatile compounds were identi ed and quanti ed using the GCMS Solution software (Shimadzu GCMS Solution V 4.45SP1). The chromatograms were analyzed rst by comparison with a blank run for background volatiles, then by comparison among the fruit VOC samples under the three treatments (SWD-attacked, physical damage, undamaged control). VOCs were identi ed from their mass spectra and retention indices, using the NIST08 and Adams' MS databases (Adams 2007) . Individual compound net amounts were calculated relative to the internal standard by peak area comparison and are hence expressed as μg int.std . / 25 g / 24 h.
Volatile compounds were identi ed and quanti ed using the GCMS Solution software (Shimadzu GCMS Solution V 4.45SP1). The chromatograms were analyzed rst by comparison with a blank run for background volatiles, then by comparison among the fruit VOC samples under the three treatments (SWD-attacked, physical damage, undamaged control). VOCs were identi ed from their mass spectra and retention indices, using the NIST08 and Adams' MS databases (Adams 2007) . Individual compound net amounts were calculated relative to the internal standard by peak area comparison and are hence expressed as μg int.std . / 25 g / 24 h.
5
Hydrodistillation and GC-MS Analysis of Essential Oils
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EOs were obtained by hydrodistillation for 3 h in a Clevenger-type apparatus and stored at 4 o C up to GC-MS, GC-FID and bioassays. Gas chromatography-flame ionization detection and gas chromatography-mass spectrometry analyses were performed by Shimadzu QP2010 Plus and GCMS2010 Plus (Shimadzu Corporation, Kyoto, Japan) systems. GC-MS and GC-FID conditions and the identification of chemical constituents of EOs were carried out in agreement with the methodology proposed by Cabral et al. (2019) .
6
GC-MS Analysis of Chemical Compounds
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GC-MS analysis were carried out on a gas chromatography-mass spectrometer QP 2010 Plus (Shimadzu, Japan) with the separation of a DB-5MS capillary column(0.25 μm, 30 m × 0.25 mm). The injector temperature was 280 °C and injection volume was 1.0 μL. Oven temperature was programmed as follows: it held at 40 °C for 1 min, and ramped to 120 °C at a rate of 40 °C/min, and increased to 280 °C at a rate of 5 °C/min, and increased to 300 °C at a rate of 12 °C/min, then held for 7 min. Helium was set as carrier gas with flow rate 0.75 mL/min. The ion source of MS was operated in the electron ionization mode (EI, 70 eV). Qualitative and quantitative analyses were based on internal standards and standard curves.
7
GC-MS Analysis of Bergamot Essential Oil
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GC-MS analysed BEO using Shimadzu QP 2010 Plus apparatus (Columbia, SC, USA) equipped with an AT WAX 30 m 0.32 mm 1 µm capillary column. The discharge rate of the carrier gas, helium, was 1 mL/min, and the temperatures of the injector and ion source were 250 °C and 220 °C, respectively. For compound separation, a temperature gradient was utilised with an initial oven temperature of 40 °C maintained for 1 min, followed by an increase to 210 °C at a rate of 5 °C/min and a subsequent 5-min hold at this temperature. The sample injection volume was 1 μL of a 2% BEO hexane solution, and a split ratio of 1:50 was utilised. The GC-MS analysis was executed in triplicate.
The volatile components of the essential oil evaluated were identified using the NIST 5 Wiley 275 library database. The match of detected compounds to the database was a minimum of 90%. The results were presented as percentages from total compounds. LRI (Linear Retention Index) was calculated using Normal alkane RI for the same polar column [19 (link)]. The values obtained refer to the percentage area of the chromatographic bands (peaks) on the chromatogram corresponding to the compounds identified.
The volatile components of the essential oil evaluated were identified using the NIST 5 Wiley 275 library database. The match of detected compounds to the database was a minimum of 90%. The results were presented as percentages from total compounds. LRI (Linear Retention Index) was calculated using Normal alkane RI for the same polar column [19 (link)]. The values obtained refer to the percentage area of the chromatographic bands (peaks) on the chromatogram corresponding to the compounds identified.
8
Quantifying Iopamidol and Its Transformation Products
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Iopamidol was quantified by using a hybrid quadrupole-orbitrap mass spectrometer (Q Exactive, Thermo Fisher Scientific Inc., Waltham, MA, USA) coupled with liquid chromatography (UltiMate 3000 LC systems, Thermo Fischer Scientific Inc.). To investigate the TPs derived from the iopamidol-containing solution during ozonation and ozonation-chlorination, their accurate masses were similarly determined by using the hybrid quadrupole-orbitrap mass spectrometer coupled with liquid chromatography. Two low-molecular-weight iodic TPs (iodoacetic acid and iodoform) were quantified by using the LC-MS/MS system (LC, UltiMate 3000 LC systems; MS/MS, Q Exactive, Thermo Fisher Scientific Inc.) and a GC-MS system (QP2010 Plus, Shimadzu Corporation, Kyoto, Japan) equipped with a capillary column (DB-1ms UI, Agilent Technologies, Palo Alto, CA, USA; length, 30 m; internal diameter, 0.25 mm; thickness, 0.25 µm), respectively. Details regarding measurements are described in Supplementary content.
9
Monosaccharide Composition Analysis of EPS
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The monosaccharide composition of EPS was analyzed by gas chromatography-mass spectrometry (GC-MS) (Shimadzu QP 2010 plus, Japan) with a flame ionization detector (FID) and an Rxi-5 Sil MS column (30 m × 0.25 mm × 0.25 μm). Briefly, 2 mg of EPS samples were hydrolyzed with 1 mL of 2 M trifluoroacetic acid (TFA) for 90 min, after which the acid was removed by evaporation. The hydrolysate was washed using milliQ water and dried. The dried hydrolysate was then reduced with sodium borohydride and acetylated using acetic anhydride (Du et al., 2018 (link)). The derivative was subjected to GC-MS analysis. Standards of rhamnose, halidose, arabinose, xylose, mannose, galactose, and glucose were prepared for composition analysis.
10
GC-MS Analysis of Plasticizers
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The method proposed by Di Bella et al. [21 (link)] was used for plasticizers determination. A gas chromatograph (GC-2010) equipped with a quadrupole mass spectrometer (QP-2010 Plus) purchased by Shimadzu Italia (Milan, Italy) was employed. A capillary column (Supelco SPB-5MS; 30 m, 0.25 mm i.d., 0.25 µm film thickness) was used for separation of analytes in the following programmed temperature: from 60 to 190 °C with a gradient of 8 °C/min, 5 min hold at 190 °C, from 190 to 240 °C a gradient of 8 °C/min, 5 min hold at 240 °C, from 240 to 315 °C with a gradient of 8 °C/min. The carrier gas was helium (5.5 purity; constant rate of 30 cm/s); the transfer line temperature was 280 °C; the injector temperature was 250 °C. Injections were performed with a splitless injector, closed for 60 s, and then with a split ratio of 1:15. The acquisition was performed from 40 to 400 m/z in full scan and in Single Ion Monitoring (with ionization energy at 70 eV and emission current at 250 µA). As reported in Table 2 , one target ion (T) and the two qualitative ions (Q1 and Q2) were used for each analyte.
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