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Gcms qp5050 spectrometer

Manufactured by Shimadzu
Sourced in Japan

The GCMS-QP5050 is a gas chromatograph-mass spectrometer (GC-MS) instrument manufactured by Shimadzu. It is designed to separate, identify, and quantify various chemical compounds in a sample. The instrument combines the separation capabilities of gas chromatography with the identification and detection capabilities of mass spectrometry.

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4 protocols using gcms qp5050 spectrometer

1

Synthesis of Cubane Derivatives via Thiolation Reactions

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Potassium tert-butoxide, 4-methoxybenzenethiol (3), benzenethiol (4), naphthalene-2-thiol (11) and potassium diphenylphosphide solution (0.5 M in THF) are commercially available and used as received. Methyl-4-iodocubane-1-carboxylate (1) and 1,4-diiodocubane (2) were synthesized according to ref. 18 (link). DMSO is Carlo Erba and stored under molecular sieves (4 Å). 1H NMR and 13C NMR spectra were recorded on a 400 MHz Bruker nuclear magnetic resonance spectrometer. HR-MS were recorded on a Bruker, MicroTOF Q II equipment, operated with an ESI source in (positive/negative) mode, using nitrogen as nebulizing and drying gas and sodium formate 10 mM as internal standard. Gas chromatographic analyses were performed on a Varian 3900 GC with flame ionization detector on a FactorFour capillary column (VF-5 MS, 30 m, 0.32 mm, 0.25 micron). GC-MS analyses were carried out on a Shimadzu GC-MS QP5050 spectrometer, employing a 30 m, 0.32 mm, 0.25 micron, DB-5 MS column. Irradiation was performed in a reactor equipped with two 400 W lamps (Philips model Master HPI-T Plus, air- and water-cooled). The Fig. SI-1 in ESI shows the spectrum of the lamps. HPLC analyses were carried out on a Waters 1525 Binary HPLC Pump connected to a Waters 2998 Photodiode Array Detector, and employing an Agilent Zorbax Eclipse XDB-C18 Analytical column (4.6 × 150 mm, 5 μm).
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2

Isolation and Characterization of Arborescen Alkaloid

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AM was extracted from the stem bark of C. arborescens, wild trees growing in Malaysia. A voucher specimen was deposited at the Herbarium, Department of Biology, University Putra Malaysia. Hexane, chloroform and methanol extracts were collected. The characterization and identification of AM have been done using JOEL ECA-400 spectrometer and mass spectra data was recorded using a Shimadzu GCMS-QP5050 spectrometer (Sidahmed et al., 2013 (link)). The purity of AM was confirmed to be 100% by HPLC-LC 20 AD (Shimadzu, Japan) using reversed-phase C18, 2.5 mm column from Waters with 10% acetonitrile in water. One peak has been observed between 7–7.5 min. The detection of the peak was at 245 nm wavelength using a Gilson absorbance detector (UV–VIS165 Gilson USA).
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3

Toluene-Based Spectroscopic Characterization

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Toluene (Carlo Erba) and
solvents in general were used after distillation and stored under
molecular sieves (4 Å) and an inert atmosphere. 1H-NMR, 13C-NMR, and all 2D NMR spectra were recorded using a 400 MHz
Bruker nuclear magnetic resonance spectrometer. HRMS spectra were
recorded using a Bruker, MicroTOF-Q II equipment, operated with an
ESI source in the positive/negative mode, using nitrogen as a nebulizing
and drying gas and 10 mM sodium formate as an internal standard. A
gas chromatographic analysis was performed using a Varian GC with
a flame ionization detector, which was equipped with a VF-5 MS, 30
m × 0.25 mm × 0.25 mm column. GC–MS analyses were
carried out on a Shimadzu GC–MS QP5050 spectrometer, employing
a 30 m, 0.12 mm DB-5 MS column.
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4

Isolation and Characterization of AM from Cratoxylum arborescens

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The stem bark of Cratoxylum arborescens was collected from wild trees growing in Malaysia. A voucher specimen was deposited at the Herbarium, Department of Biology, University Putra Malaysia. The finely ground air-dried stem bark of Cratoxylum arborescens (1.0 kg) was extracted consecutively with hexane, chloroform, and methanol to produce 6.12, 28.18, and 40.27 g, respectively, of dark, viscous semisolid material upon solvent removal. The hexane extract was chromatographed over a vacuum column and eluted with a solvent of gradually increasing polarity to produce 26 fractions of 200 mL each. This extensive fractionation and purification of fractions 14–20 consequently yielded 160 mg (26.14%) of AM (Figure 1). The characterization and identification of AM were performed and proven using a JOEL ECA-400 spectrometer (JOEl, Tokyo, Japan) operating at 400 MHz and 100 MHz for 1H and 13C, respectively. Mass spectra data was recorded using a Shimadzu GCMS-QP5050 spectrometer (Shimadzu Co., Ltd., Kyoto, Japan). The retention time was between 7–7.5 min. One peak was observed for 15 min. The detection of the peak was performed at a wavelength of 245 nm with a Gilson absorbance detector (UV-VIS165 Gilson, Middleton, Wisconsin, USA) (Figure S1).
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