Products were analysed as Me/TMS derivatives by GC–MS. The GC–MS analyses were performed using a Shimadzu QP5050A mass spectrometer connected to a Shimadzu GC-17A gas chromatograph equipped with a Supelco MDN-5S (5% phenyl, 95% methylpolysiloxane)-fused capillary column (length, 30 m; ID 0.25 mm; film thickness, 0.25 μm). Helium at a flow rate of 30 cm/s was used as the carrier gas. Injections were made in split mode using an initial column temperature of 120 °C and injector temperature 230 °C. The column temperature was raised at 10 °C/min until 240 °C. The electron impact ionization (70 eV) was used. Most GC–MS analyses were carried out in full-scan mode. The NMR 1H, 1H-1H-COSY, 1H-13C-HSQC, 1H-13C-HMBC, 1H-1H-NOESY and 1H-1H-TOCSY spectra ([2H14]n-hexane) were recorded on a Bruker Avance III 600 spectrometer at 253 K.
Qp5050a mass spectrometer
Manufactured by Shimadzu
Sourced in Germany, United States
The QP5050A mass spectrometer is an analytical instrument designed for the detection and identification of chemical compounds. It utilizes mass spectrometry technology to precisely measure the mass-to-charge ratio of ionized molecules, providing detailed information about their molecular structure and composition.
Automatically generated - may contain errors
Lab products found in correlation
Mdn 5s, by Merck Group (1 mentions)
Gc 17a gas chromatograph, by Merck Group (1 mentions)
Avance 3 600 spectrometer, by Bruker (1 mentions)
Db 5 column, by Merck Group (1 mentions)
Drx500, by JEOL (1 mentions)
Eclipse 400, by JEOL (1 mentions)
Db 5ms, by Agilent Technologies (1 mentions)
Gc 17a gas chromatograph, by Shimadzu (1 mentions)
Tlc silica gel 60 f254, by Merck Group (1 mentions)
Gc 17a, by Shimadzu (1 mentions)
Avance 3 600, by Bruker (1 mentions)
Spd m20a diode array detector, by Shimadzu (1 mentions)
7 protocols using qp5050a mass spectrometer
1
Analyzing Compounds via GC-MS and NMR
2
GC/MS Analysis of Coffee Volatiles
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GC/MS analysis of coffee volatiles was performed exactly as previously described by Farag et. al. [17 (link),18 (link)]. Three biological replicates were analyzed for each specimen, using a Shimadzu GC-17A gas chromatograph equipped with a DB-5 column (30 m, 0.25 mm × 0.25 um film thickness; Supelco®, Merck SA, Darmstadt, Germany) coupled to a Shimadzu QP5050A mass spectrometer.
3
Spectroscopic Analysis of Chemical Compounds
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Measures of optic rotation were obtained on a Perkin Elmer 343 digital polarimeter. Melting point was obtained on a Microquímica MQRPF. EI-MS (low resolution) mass spectra were obtained on Shimadzu QP5050A mass spectrometer. HRESI-MS (high resolution) mass spectra were obtained by using a ESI-IT-OF-MS SHIMADZU mass spectrometer, using the positive ion mode of analysis. Chromatographic purifications were carried out over silica gel 60 (70–230 mesh). Silica gel 60 F254 was used in thin layer chromatography analysis. 1H and 13C-NMR spectra were measured on a Bruker model DRX-500 and Jeol model Eclipse-400 spectrometers, equipped with inverse probes and field gradient, operating at 500 (1H) and 125 (13C) and 400 (1H) and 100 (13C) MHz. CDCl3 and pyridine-d5 were used as solvents and TMS as internal reference. Chemical shifts are given in the δ scale (ppm) and coupling constants J in Hz. One dimensional (1D) 1H and 13C-NMR spectra were acquired under standard conditions by using a direct detection 5 mm 1H/13C dual probe. Standard pulse sequences were used for two dimensional spectra by using a multinuclear inverse detection 5 mm probe with field gradient.
4
GC-MS Analysis of Organic Compounds
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A GC-17A gas chromatograph (Shimadzu, Coppell, TX, USA) attached to a GC-MS QP 5050A Mass Spectrometer (Shimadzu) with a GC-MS electron impact ionization method was used. A fused silica capillary column (DB-5 ms-J&W) with dimensions of 30 m × 2.5 mm, 0.25 mm was employed. The conditions for the GC-MS run are as follows: the injection temperature and the interface temperature were kept at 300 °C while the ion source was adjusted to 250 °C, with helium as the carrier gas at a flow rate of 1 mL/min. Isothermal heating at 100 °C (1 min) followed by 300 °C for 20 min was used. The mass spectra were quantified by studying the peak areas and referring to the internal standard.
5
Silica Gel Purification and Analysis
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All reagents and solvents used were analytical grade. Column chromatography was performed with Merck 7734 (0.040–0.063 mm) or Merck 9385 (0.063–0.200 mm) silica gel, while elutes were analyzed with Merck TLC silica gel 60 F254. Nuclear magnetic resonance (NMR) was recorded in CD3OD or CDCl3 using a 500 MHz Varian spectrometer, and mass analysis was done with a Shimadzu QP5050A mass spectrometer. Melting points were determined using a Fisher–Johns hot stage melting point apparatus equipped with microscope.
6
Spectroscopic Analysis of Organic Compounds
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UV spectra were recorded online during the HPLC separations with a SPD‐M20A diode array detector (Shimadzu). GC–MS analyses were performed by using a Shimadzu QP5050A mass spectrometer connected to a Shimadzu GC‐17A gas chromatograph equipped with an MDN‐5S (5 % phenyl, 95 % methylpolysiloxane) fused capillary column (length, 30 m; inner diameter, 0.25 mm; film thickness, 0.25 μm). Helium at a flow rate of 30 cm s−1 was used as the carrier gas. Injections were made in the split mode by using an initial column temperature of 120 °C. The temperature was raised at 10 °C min−1 until 240 °C. Full‐scan GC–MS analyses were performed by using an ionization energy of 70 eV. The 1H NMR, 1H–1H COSY, 1H–1H TOCSY, 1H–1H NOESY, 1H–13C HSQC, and 1H–13C HMBC spectra were recorded with a Bruker Avance III 600 instrument (600 MHz, [2H6]benzene, 296 K).
7
Metabolite Analysis of Seed Extracts
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The analysis of primary metabolites was conducted as described in19 (link). In brief, the finely powdered seeds (100 mg) were extracted with methanol and centrifugated at 12,000 rpm for 10 min to get rid of the debris. Samples were sonicated and extracted once, following the same protocol as20 (link),21 (link).
Three samples of each seed were analysed using the same conditions to consider the biological variation. The methanol extracts were evaporated under a nitrogen gas stream till dryness. Dried pellet was derivatized using 150 µL of N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA) and incubated for 45 min at 60 °C. GC/MS analysis was carried out on a Shimadzu GC-17A gas chromatograph that is coupled to Shimadzu QP5050A mass spectrometer, using Rtx-5MS column (30 m length, 0.25 mm inner diameter, and 0.25 μm film thickness).
Three samples of each seed were analysed using the same conditions to consider the biological variation. The methanol extracts were evaporated under a nitrogen gas stream till dryness. Dried pellet was derivatized using 150 µL of N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA) and incubated for 45 min at 60 °C. GC/MS analysis was carried out on a Shimadzu GC-17A gas chromatograph that is coupled to Shimadzu QP5050A mass spectrometer, using Rtx-5MS column (30 m length, 0.25 mm inner diameter, and 0.25 μm film thickness).
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