Quantitative analysis of the reaction component (DiTMP) was performed using gas chromatography (GC, Varian 430-GC, Varian, USA) equipped with FactorFour Capillary column, VF-1ms (Varian, 15M × 0.25mm) and a flame ionization detector. The initial column temperature was increased from 50 °C to 250 °C at a rate of 20 °C/min. The samples, diluted with acetonitrile, to a concentration of 0.01–0.5 mg/mL, were injected in a split injection mode of 10% at 275 °C. About 10 mg of samples was taken from the reactant during time course, and was dissolved at 10 mg/mL concentration in acetonitrile at room temperature for 20 min. After the solution was centrifuged at 12,000 rpm for 1 min, the resulting supernatant was injected to measure the remaining monomer to GC (Fig. S2 ). The residual amount and conversion rate of DTMPC in the reaction were calculated by using standard curves of DTMPC concentration. All the data were obtained from two independent experiments and were provided as the average of the replicates with error bars.
Vf 1ms
Manufactured by Agilent Technologies
Sourced in United States
The VF-1ms is a capillary column designed for gas chromatography (GC) applications. It features a 100% dimethylpolysiloxane stationary phase, which provides high-temperature stability and excellent inertness for the analysis of a wide range of compounds. The column is available in various lengths and internal diameters to suit different analytical requirements.
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Lab products found in correlation
6 protocols using vf 1ms
1
Quantitative Analysis of DiTMP by GC
2
Styrene Epoxidation Catalyzed by Cu@dppz-vPMO
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Epoxidation reaction of styrene was carried out in a two necked round-bottom glass reactor equipped with a magnetic stirring bar and a reflux condenser. Toluene and nitrobenzene were used as solvent and internal standard, respectively [24] (link). Typically, 50 mg of catalyst was added to a solution containing styrene (0.058 mL, 0.5 mmol), tertbutyl hydroperoxide (TBHP, 0.2 mL, 0.5 mmol), nitrobenzene (0.082 mL, 0.8 mmol) and toluene (2 mL). Afterwards, the reaction mixture was kept under stirring at 90 ºC for 1 h. Sample aliquots (0.2 mL) were taken out from the mixture and diluted with toluene. The products were analysed and quantified in a Varian gas chromatograph with a capillary column (VF-1MS, 15 m x 0.25 mm ID) and a flame ionization detector (FID) and using standard compounds. After the reaction, the catalyst was filtered off, washed with acetonitrile and dried under vacuum at 90 ºC, and then reused directly without further purification. The recyclability of the Cu@dppz-vPMO catalyst was investigated during five consecutive runs.
One blank reaction was carried out without adding any catalyst under the same experimental conditions.
One blank reaction was carried out without adding any catalyst under the same experimental conditions.
3
Separation of Trichothecenes by GC-ECD
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Separation of trichothecenes, nivalenol, and fuzarenone X was carried out using a Varian CP-3800 gas chromatograph (Varian Medical Systems, Palo Alto, CA, USA) equipped with an detector ECD (instant connect Electron Capture Detector) and columns VF-1ms 30 m × 0.32 mm ID (Column Internal Diameter), DF (film thickness) = 0.25 µm from Varian. The temperature of the dispenser chamber was 250 • C and the detector 300 • C. The following oven temperature gradient was used: 80 • C for 1 min, increment 40 • C for 1 min to 160 • C, 3 • C for 1 min to 178 • C, 2 • C for 1 min to 240 • C, 40 • C for 1 min to 270 • C, 270 • C for 1 min. Nitrogen was used as carrier gas at a flow rate of 1 mL for min.
4
Synthesis of Ortho-Isoprenylated Phenols
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The conditions for the GC assays were Column: VF-1ms (Varian Inc. 30m x 0.255mm) with helium as carrier gas. Oven temperature program was 70 • C (3 min), 10 • C/min to 310 • C and hold for 6 min.
General procedure for ortho-isoprenylated phenol synthesis 1.1 equivalents of the phenol substrate were dissolved in anhydrous toluene at 0 • C. Then, 0.3 equivalents of BF 3 •Et 2 O were added followed by the addition of 1 equivalent of the corresponding isoprenol. After 12 h of continuous stirring at 4 • C, the reaction was quenched with saturated NaHCO 3 . The inorganic phase was extracted 3 times with AcOEt and the combined organic layers concentrated under vacuum. The residue was purified on a silica gel column (Hexane-AcOEt gradient).
General procedure for ortho-isoprenylated phenol synthesis 1.1 equivalents of the phenol substrate were dissolved in anhydrous toluene at 0 • C. Then, 0.3 equivalents of BF 3 •Et 2 O were added followed by the addition of 1 equivalent of the corresponding isoprenol. After 12 h of continuous stirring at 4 • C, the reaction was quenched with saturated NaHCO 3 . The inorganic phase was extracted 3 times with AcOEt and the combined organic layers concentrated under vacuum. The residue was purified on a silica gel column (Hexane-AcOEt gradient).
5
Gas Chromatography-Mass Spectrometry Protocol
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Analyses were performed with an Agilent 5975N (Agilent Technologies) using MS/FID (Agilent MSD5975) detector, a 100% polydimethylsiloxane (Agilent VF-1MS) (0.25 µm × 0.25 mm × 60 m) as the stationary phase, with Helium as the mobile phase, over 95 min, 1 mL/min, column temperature: 250 °C, sample volume injection: 0.5 μL.
6
Hexadecane Extraction and Quantification Protocol
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Hexadecane extraction and quantification was performed according to Castro et al. (2016) . Briefly, hexadecane in the culture medium was sequentially extracted from each replicate flask (total content of the flask analyzed) in a separation funnel using hexane as solvent. Hexadecane concentration was determined in a gas chromatograph coupled to a flame ionization detector (GC-FID) (GC Varian® star 3400CX, USA). The column used was the model VF-1 ms (Agilent, USA) 30 m length long × 0.025 mm internal diameter, made from fused silica coated with dimethylpolysiloxane as stationary phase. Helium was used as carrier gas at a flow rate of 1 mL min -1 . The temperature of the detector and the injector were set at 300 and 285 °C, respectively. The column's temperature was maintained at 60 °C for 1 min and then raised up to 290 °C at a rate of 8 °C min -1 .
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