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11 protocols using 6890n chromatograph

1

GC-MS Analysis of L. dulcis Essential Oils

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The L. dulcis EOs were qualitatively analyzed by GC-MS using an Agilent Technologies Chromatograph 6890N coupled to an Agilent mass spectrometer, the 5973 Inert series (Santa Clara, CA, USA), which operated in electron impact mode at 70 eV. The mass spectrometer was operated in SCAN mode (range 35–350 m/z), had a scan rate of 0.2 scan/s, and was controlled by MSD-Chemstation D.01.00SP1.
The reported results of the EOs analysis were obtained on a DB-5ms (5% phenyl-polymethylsiloxane; 30 m × 0.25 mm × 0.25 µm, Agilent Technologies; J; W Scientific, Folsom, CA, USA) capillary column; helium (1.00 mL/min) was used as the carrier gas. The injection system operated in split mode (40:1) at 220 °C. The program for the GC oven temperature was as follows: initial temperature of 60 °C, held for 5 min, followed by a ramp of 3 °C/min until 250 °C, which was finally held for 10 min. Each EO was diluted with CH2Cl2 (1:100 v/v), and 1 μL of the solution was injected into each analysis.
To calculate LRIs, a homologous series of n-alkanes C9–C25 (C9, BHD purity 99%, and C10–C25, Fluka purity 99%) were injected after each EO under identical chromatographic conditions.
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2

GC-MS Analysis of Essential Oil

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The EO was qualitatively analysed by GC-MS, using an Agilent Technologies Chromatograph 6890N, coupled to an Agilent mass spectrometer, 5973 Inert series, which operated in electron impact mode at a 70 eV and was controlled by an MSD-ChemStation software.
Two types of chromatographic columns were used for the analysis: a non-polar column DB-5ms (5% phenyl-methylpolysiloxane; 30 m × 0.25 mm × 0.25 µm) and a HP-INNOWax polar column (polyethylene glycol; 30 m × 0.25 mm × 0.25 µm); helium was used as the carrier gas in both analyses (at a constant flow of 1.00 mL/min). The injection system operated in split mode (40:1) at 220 °C. The GC oven temperature was programmed at 60 °C (5 min), then it was increased to 250 °C (10 min) at a rate of 3 °C/min. We injected 1 μL of a solution of the EO in CH2Cl2 (1:100 v/v) in each analysis.
The volatile components of the EO were identified by comparing the linear retention indices (LRI) and the mass spectra with the data reported in the literature. Each LRI was calculated according to Van Den Dool and Kratz [27 (link)], from a homologous series of n-alcanes C9–C25 (C9, BHD purity 99% and C10–C25, Fluka purity 99%), which were injected on each of the two columns after the EO, under identical conditions [17 (link)].
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3

Fatty Acid Profiling by Gas Chromatography

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The fatty acids content was determined by gas chromatography (GC) by means of an Agilent Technologies chromatograph 6890 N model fitted with a TR-CN100 capillary column (60 m length × 0.25 mm internal diameter × 0.20 μm thickness) and a flame ionization detector. The injector and detector temperatures were 280 °C and 260 °C, respectively. The oven temperature was 185 °C. The carrier gas used was hydrogen at the rate of 38.02 cm/s, and air and hydrogen were used as auxiliary gases [43 (link)].
The fatty acids were identified by comparing the retention times of the borage methyl esters against those of known mixtures of standard fatty acids (Sigma-Aldrich, Barcelona, Spain) after processing them with the same column under the same conditions.
A preliminary step was required prior to injecting the oil into the GC for the individual determination of its fatty acids content. The fractions obtained were converted into their corresponding methyl ester (FAME) [44 (link)].
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4

GC-MS Analysis of Tarragon Oil

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The analysis of Artemisia dracunculus essential oil by gas chromatography was carried out using an Agilent 6890N Chromatograph equipped with a flame ionization detector (FID) and an Agilent 5975 inert XL mass detector (MSD) with an ionization energy of 70 eV. Two Teknokroma TR-520232 capillary columns were used. The analysis conditions were: an initial temperature of 40 °C for 14 min; a gradient of 1.5 °C/min up to 250 °C; and an isotherm for 10 min. The injector (and transfer line) temperature was 270 °C. Helium was used as a carrier gas for the 2 L of injected Artemisia dracunculus essential oil in splitless mode at a flow rate of 0.5 mL/min. GC-MS analysis was performed by ESI in a mass range of 24 to 400 m/z with a delay time of 2 min. Identification of Artemisia dracunculus components was performed by comparing the mass spectra to those in the available NIST database (GC-MS) and by their relative retention index (Kovacs Index, KI) towards a mixture of alkanes C4 to C26, injected in the same experimental conditions (GC-FID).
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5

Catalytic Oxidation of Propane over Ru/TiO2

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The catalytic tests were carried out in a tubular reactor with porous plate (ID = 1 cm; L = 35 cm) and prior to the catalytic tests, the samples underwent an activation process at 300 and 500 °C under H2 flow (1 mg = 1 mL min−1). Flow mass controllers were used to set the flow of a gas mixture at 5000 ppm of C3H8 (purity of 99.998%) and 2% of O2 in N2 (purity of 99.997%) with a total flow rate of 100 mL min−1. The catalyzed reaction was performed using 40 or 80 mg of Ru/TiO2 catalyst, from room temperature to 500 °C, with a heating ramp of 3 °C min−1. The effluents were analyzed by gas chromatography in an in-situ Research Rig-150 equipment; the effluent analysis was performed using an Agilent Technologies 6890N chromatograph with CO, CO2, and C3H8 detection. Propane conversion (%) = ([C3H8]in − [C3H8]out/[C3H8]in) × 100.
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6

GC-MS Analysis of JALEx Compound

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JALEx was analyzed by gas chromatography combined with mass spectrometry (GC-MS) using an Agilent 6890N chromatograph (Palo Alto, CA) equipped with a capillary column DB-H17HT (30 m × 0.25 mm × 0.15 μm film thickness). Helium was the carrier gas at 1.0 mL/min and inlet pressure of 3.14 psi, 10:1 split/splitless ratio. The oven temperature was programmed from 150°C to 340°C at 4°C/min for 17 minutes. The injection volume was 1 μL of a 2 mg/mL chloroform solution. Data were processed using MSD Productivity Chem Station Software operating with ion source at 250°C and electron impact ionization at 70 eV. Individual components were characterized by their fragmentation patterns in the mass spectrum.
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7

Synthesis of Zinc-based Complexes

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Ethylzinc benzoate,5e [(EtZn)2Zn(OAr)4],7 (link)N-(4-methoxy-benzylidene)aniline (1a), N-benzylidene-4-methoxyaniline (1b)17 and tBu2Zn,18 (link) were prepared according to the literature procedures under a nitrogen atmosphere using standard Schlenk techniques. All other reagents were of commercial grade obtained from Sigma-Aldrich Co. The solvents and propionic acid used for preparation of the initiators were carefully dried and distilled under a nitrogen atmosphere prior to use. TEMPO was sublimated and stored under a nitrogen atmosphere. Oxygenation reactions were carried out using atmospheric air dried by passing it through a tube filled with anhydrous CaCl2/KOH. NMR spectra were acquired on a Varian Mercury 400 Spectrometer, and IR spectra were recorded on a Perkin-Elmer System 2000 FT-IR spectrophotometer. GC-MS analysis was performed on an Agilent 6890N chromatograph coupled with an Agilent 5973N MS detector.
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8

Lipid Composition Analysis of Ginseng Extract

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Total lipids in the ethanol extract, supernatant, and precipitate from water fractionation were determined using the procedure described by Folch et al [15] (link). The lipid composition of GEF was analyzed by hydrolyzing GEF from ginseng with 6N HCl for 4 h at 100°C or by digesting lipoprotein lipase to confirm lipid and hydrophobic moiety. Acid hydrolyzed or digested GEF was partitioned between distilled water and n-butanol (BuOH). The n-BuOH layer, after concentration, was partitioned further between distilled water and n-hexane. The n-hexane layer was prepared for lipid and hydrophobic moiety analysis using a 6890N GC–MS system (Agilent, Santa Rosa, CA, USA) with a DB5-MS capillary column (30 cm × 250 μm × 0.25 μm) at the Korea Basic Science Institute and by gas chromatography using an Agilent 6890N chromatograph equipped with a flame ionization detector and a split injection system fitted with a Supelco SPB-1 capillary column (15 m × 0.32 mm inside diameter, 0.25 mm thickness) [11] (link).
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9

Permethrin Quantification by GC-FID

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The extracts were analysed using an Agilent 6890 N chromatograph fitted with a 30 m × 0.25 mm (i.d.) fused silica DB-1 capillary column coated with 0.25 μm cross linked polydimethylsiloxane stationary phase. Ultra-high purity nitrogen (1.2 ml/min) was used as the carrier gas. Injector port, column oven, and detector temperatures were 265 °C, 240 °C, and 300 °C, respectively. Flame ionization (FID) was used for analyte detection. Two injections were used for each sample and the results averaged. Permethrin concentration was calculated by comparing permethrin/triphenyl phosphate peak area ratios against a calibration curve generated from solutions containing known permethrin /triphenyl phosphate mass ratios.
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10

Fungal Morphology and Molecular Analyses

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Fungal morphological characters were measured using a light microscope at 1000× and photomicrographs were captured with a Nikon DS-L3 camera adapted to a Nikon 80i microscope (Nikon Corp. Mitsubishi, JP). PCR products were purified and sequenced by Macrogen (Seoul, Korea). DNA was amplified using a GeneAmp 9700 DNA Thermal Cycler (PerkinElmer, Life Technology, Carlsbad, CA, USA).
The IR spectrum was recorded with a Nicolet 8700 FTIR spectrometer (Thermo Electron, Madison, WI, USA). Gas chromatography–mass spectrometry (GC-MS) analyses were done with an Agilent Technologies (Santa Clara, CA, USA) 6890N Chromatograph coupled to an Agilent 5975B mass-selective detector as previously described [5 ]. Low- and high-resolution MS spectra were recorded on a GC Mate II mass spectrometer in FAB [+] mode using NBA matrix and JEOL Calibration Ultramark and Resolution 3000 (JEOL, Peabody, MA, USA). 1H and 13C NMR spectra were recorded in an AMX-400 spectrometer (Bruker Corp., Billerica, MS, USA) at 400 and 100 MHz, respectively, using TMS as an internal standard, and in a Varian, Agilent AR Premium Compact (Varian, Palo Alto, CA, USA) at 599.774 and 150.826 MHz, respectively. Chemical shifts were reported in ppm and coupling constants (J) were given in Hz. Two-dimensional experiments (COSY, DEPT, HSQC, and HMBC) were done using the Varian equipment.
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