Melting points were determined using a MQAPF-307 melting point apparatus (Microquimica, Brazil) and remained uncorrected. The progress of the reactions was monitored by thin layer chromatography (TLC) in silica gel plates. Column chromatography was performed over silica gel (60–230 mesh). Infrared spectra were recorded on a Spectra One Perkin-Elmer spectrophotometer, fitted with a Paragon ATR accessory. Mass spectra (HRMS) were recorded on a Shimadzu GC MS-QP5050A instrument using direct insertion together with the electrospray ionization method and a quadrupole analyzer. The 1H, 13C, and DEPT 135 nuclear magnetic resonance (NMR) spectra and two dimensional NMR spectra—correlations spectroscopy (COSY), heteronuclear single-quantum correlation (HSQC), and heteronuclear multiple bound correlation (HMBC)—were recorded on a Bruker Avance DPX 200 and a DPX 400 spectrometer at 200 and 400 MHz using CDCl3 and DMSOd6 as the solvent and Tetramethylsylane (TMS) as the internal standard, unless otherwise stated. The NMR data are presented as follows: chemical shift in ppm, multiplicity, number of protons, J in Hz, and proton assignments. Multiplicities are indicated by the following abbreviations: s (singlet), d (doublet), dd (double doublet), t (triplet), q (quartet), m (multiplet), qn (quintet), st (sextet), ht (heptet), and bs (broad singlet).
Gcms qp5050a
Manufactured by Shimadzu
Sourced in Japan, United States, Italy
The GCMS-QP5050A is a gas chromatograph-mass spectrometer (GC-MS) system manufactured by Shimadzu. It is a versatile analytical instrument used for the identification and quantification of a wide range of chemical compounds. The system combines the separation capabilities of gas chromatography with the high-sensitivity detection and structural analysis capabilities of mass spectrometry.
Automatically generated - may contain errors
Lab products found in correlation
Gc 17a, by Shimadzu (5 mentions)
400 mhz spectrometer, by Bruker (4 mentions)
Dpx 400 spectrometer, by Bruker (3 mentions)
Gladi atr, by Agilent Technologies (2 mentions)
660 ir spectrophotometer, by Agilent Technologies (2 mentions)
Gcms qp2010 ultra, by Shimadzu (2 mentions)
Avance dpx 200, by Bruker (1 mentions)
Lcms 8040, by Shimadzu (1 mentions)
Gc 17a gas chromatograph, by Shimadzu (1 mentions)
Supelco spbtm 5, by Merck Group (1 mentions)
Cdcl3, by Merck Group (1 mentions)
Q exactive, by Thermo Fisher Scientific (1 mentions)
Formamide, by Merck Group (1 mentions)
Adenine, by Merck Group (1 mentions)
Avance 3 500 spectrometer, by Bruker (1 mentions)
Db 1 column, by Shimadzu (1 mentions)
D8 venture photon 100 cmos diffractometer, by Bruker (1 mentions)
Flash ea 1112 elemental analyzer, by Thermo Fisher Scientific (1 mentions)
Kieselgel 60, by Merck Group (1 mentions)
Dmso d6, by Bruker (1 mentions)
37 protocols using gcms qp5050a
1
Characterization of Organic Compounds
2
GC-MS Analysis of Leaf Surface Metabolites
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Drops of water applied to the leaf surface were collected (total 3~5 mL) and lyophilized. The dry residue was dissolved in methanol (100 μL) and directly analyzed by GC-MS (Shimadzu GCMS-QP5050A) using a TC-FFAP capillary column (30 m × 0.25 mm). The GC was temperature programmed with an initial 1 min at 200°C, then a rise of 10°C/min to final isothermal period at 280°C. Detector temperature was set at 250°C. For quantitative determination, standard n-octadecanal was synthesized from commercially available n-octadecanoic acid (Wako Chemicals) by reduction with diisobutylaluminum hydride. The structure was confirmed by H-NMR (Bruker AVANCE III 400) and ESI-MS (Shimadzu LCMS-8040).
3
Gas Chromatography-Mass Spectrometry Analysis of Essential Oils
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Essential oils were chemically analyzed [25 (link)] within two months of their production date. Ten microliter of each essential oil sample was added into a clear screw-top GC-vial (6.0 mm diameter, silicone septa, 2 mL volume), and then 1.5 mL of dichloromethane was added to each vial. A blank containing only dichloromethane was included to confirm its purity. Essential oils were analyzed using a gas chromatography apparatus equipped with a quadruple mass spectrometer (GC-MS) (Shimadzu, GC-MS-QP/5050A). A nonpolar capillary column (DB-5MS, thickness; 0.25 μm, length; 30 m, internal diameter; 0.25 mm) was used to separate the components of the essential oils using a splitless mode. The temperature was kept at 51 °C for 1 min and then raised to 211 °C at a rate of 3 °C min−1. The injector temperature was 275 °C, and the interface temperature was 300 °C. Helium was used as the carrier gas. Chemical compounds were identified by matching their fragmentation patterns in the resultant mass spectra with those stored in the computer’s mass spectral database.
4
GC-MS Analysis of Essential Oil
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To obtain the chromatographic profile of the essential oil a Shimadzu GC-17A Gas Chromatograph (Shimadzu, Milan, Italy) equipped with a 15 m × 0.1 mm × 0.1 mm fused silica capillary column (Supelco SPBTM-5, Merk KGaA, Darmstadt, Germany) and Flame Ionization Detector (FID) was used. GC-MS analyses were performed on a Shimadzu GCMS-QP5050A (Shimadzu, Milan, Italy). The operating conditions for both runs were the following: 60 °C for 1 min, 60–280 °C at 10 °C/min then 280 °C for 1 min; injector temperature 250 °C; detector temperature 280 °C; carrier gas helium (1 mL/min); split mode (1:200), the volume of injection 1 mL (4% essential oil/CH2Cl2v/v). Percentages of compounds were determined from their peak areas in the GC-FID profiles. Mass spectrometer parameters were the following: Ionization at 70 eV, ion source temperature 180 °C. Mass spectral data were acquired in the scan mode in m/z range 40–400. Oil solutions were injected with the split mode (1:96) [40 (link)].
The identity of components was based on their retention index relative to C9–C22n-alkanes on the SPBTM-5 column and computer matching of spectral MS data with those from NIST MS 107 and NIST 21 libraries [41 ], the comparison of the fragmentation patterns with those reported in the literature [42 ].
The identity of components was based on their retention index relative to C9–C22n-alkanes on the SPBTM-5 column and computer matching of spectral MS data with those from NIST MS 107 and NIST 21 libraries [41 ], the comparison of the fragmentation patterns with those reported in the literature [42 ].
5
Purification and Characterization of Organic Compounds
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All compounds were purified by silica-gel column chromatography and recrystallization from diethyl ether. Reaction progress was followed by visualizing thin layer chromatography (TLC) plates with the spotted reaction mixture and starting material solution in an ultraviolet (UV) chamber [21 (link)]. The plates were then chemically stained with vanillin spray reagent.
Melting points were obtained on an MQAPF-301 (Microquímica Equipamentos Ltda, Palhoça, Brazil) melting point apparatus and were not corrected. Infrared (IR) spectra were acquired using a Varian 660-IR spectrophotometer (equipped with GLADI-ATR, Agilent, Santa Clara, CA, USA) with the attenuated total reflectance (ATR) method. NMR spectra were performed on a Brucker Avance DRX 400 MHz equipment (Billerica, MA, USA), using CDCl3 (Sigma-Aldrich, São Paulo, Brazil) as solvent. Chemical shifts were reported using tetramethylsilane (TMS) signals (δ = 0.0 ppm) as reference. The mass spectra were obtained on a Shimadzu equipment (Kyoto, Japan) GC-MS-QP5050A and GC-MS-QP2010 Ultra, after electron impact ionization (EI) at 70 eV. The NMR, IR, and mass spectra of the synthesized compounds can be found in theSupplementary Material .
Melting points were obtained on an MQAPF-301 (Microquímica Equipamentos Ltda, Palhoça, Brazil) melting point apparatus and were not corrected. Infrared (IR) spectra were acquired using a Varian 660-IR spectrophotometer (equipped with GLADI-ATR, Agilent, Santa Clara, CA, USA) with the attenuated total reflectance (ATR) method. NMR spectra were performed on a Brucker Avance DRX 400 MHz equipment (Billerica, MA, USA), using CDCl3 (Sigma-Aldrich, São Paulo, Brazil) as solvent. Chemical shifts were reported using tetramethylsilane (TMS) signals (δ = 0.0 ppm) as reference. The mass spectra were obtained on a Shimadzu equipment (Kyoto, Japan) GC-MS-QP5050A and GC-MS-QP2010 Ultra, after electron impact ionization (EI) at 70 eV. The NMR, IR, and mass spectra of the synthesized compounds can be found in the
6
GC-MS and GC-FID Analysis of Essential Oils
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Gas chromatography–mass spectrometry (GC–MS) and gas chromatography with flame ionization detector (GC–FID) analyses were performed on a Shimadzu GC-MSQP-5050A and GC-17A equipped with a DB-1 fused silica column (60 m × 0.25 mm i.d., 0.25 µm film thickness), with an oven temperature of 50 °C rising to 260 °C at a rate of 3 °C/min. The total running time for a sample was about 82 min. Helium was used as the carrier gas at a flow rate of 1.3 mL/min. The essential oil was diluted 1:100 in n-hexane and 1 µL was injected into the column. Split ratio, ionization energy, scan time, and acquisition mass range were 1:33, 70 eV, 1 s, and 30–600 amu, respectively.
7
Analytical Characterization of Meteorite Sample NWA 1465
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Formamide, D-ribose, 2-D-deoxyribose and adenine were purchased from Aldrich. NWA 1465 was obtained from Sahara-nayzak, Asnieres sur Seine, France. Gas-chromatography mass-spectrometry (GC-MS) analyses were performed with a LC/GG MS Combo Agilent and Shimadzu GC-MS QP5050A with a Variant CP8944 column (WCOT fused silica, film thickness 0.25 μm, stationary phase VF-5ms, Øί 0.25 mm, lenght 30 m). UHPLC were performed on Ultimate 3000 Rapid Resolution system (DIONEX, Sunnyvale, USA) using Reprosil C18 column (2,5 μm × 150 mm × 2.0 mm). MALDI were performed on Q-Exactive (Thermo). NMR spectra were acquired with a Bruker Avance III 500 spectrometer. Computations were carried out at B3LYP/6-31 + G* level within the COSMO continuum solvent approximation.
8
GC-MS Analysis of Oregano Essential Oil
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Gas chromatographic (GC) analysis of the O. vulgare ssp. hirtum essential oil was conducted using a GC-17A gas chromatograph (Shimadzu, Milan, Italy) equipped with a fused silica ca-pillary column (Supelco SPBTM-5 15m, 0.1mm, 0.1mm, Merck KGaA, Darmstadt, Germany) and Flame Ionization Detector (FID) as the detector. GC–MS analyses were performed on GCMS-QP5050A (Shimadzu, Milan, Italy) The operating conditions for both runs were the following: 60 °C for 1 min, 60–280 °C at 10 °C/min then 280 °C for 1 min; injector temperature 250 °C; detector temperature 280 °C; carrier gas helium (1 mL/min); volume of injection 1 μL (4% essential oil/CH2Cl2v/v). Percentages of compounds were determined from their peak areas in the GC-FID profiles. Mass spectrometer parameters were the following: ionization at 70 eV, Ion source temperature of 180 °C. Mass spectral data were acquired in the scan mode in m/z range 40–400. Oil solutions were injected into the split mode (1:96) [74 (link)]. The identity of components was based on their retention index relative to C9–C22n-alkanes on the SPB-5 column and computer matching of spectral MS data with those from NIST MS 107 and NIST 21 libraries [75 ], the comparison of the fragmentation patterns with those reported in the literature [76 (link)].
9
Pyrolysis Analysis of Riparin I
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Pyrolysis studies were conducted by a pyrolyzer coupled with a gas chromatograph system (Shimadzu, GCMS-QP5050A), which interfaced directly with a mass spectrometer using electron ionization source. The fragmentation was performed by electronic impact with an ionization energy of 70 eV. The spectrometer was operated in scan mode, sweeping a mass range of m/z 50–600. The temperature of the ion source was 300 °C. A capillary column 30 m long, with 0.25 mm internal diameter and 0.25 µm particle size, was used with stationary phase phenyl:dimethylpolysiloxane (5:95). The temperature program of the column raised the temperature at a heating rate of 15 °C min−1 up to a final temperature of 280 °C. Helium was used as the carrier gas at a flow rate of 1.0 mL min−1 with a split ratio of 1:5. The samples corresponding to a powder of riparin I batches were put in a platinum crucible and introduced into the pyrolyzer at the temperatures of 250 and 500 °C for each experiment.
10
GC-MS Analysis of n-Hex Extract
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1 μL of the n-Hex extract and its fractions were injected into the apparatus of Shimadzu GCMS-QP5050A equipped with a DB-1 column (60 m × 0.25 mm; film thickness 0.25 μm). The initial oven temperature was 50 °C for 3 minutes that raised to 270 °C at a rate of 4 °C/min finally the injection temperature was set up at 240 °C according to the described method by [24 (link), 25 (link)].
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