Aoc 5000 plus

Solutions of a commercial petrodiesel sample and the bio-oils were prepared at 10.0 mg mL⁻¹ in n-hexane, and analyzed using a Shimadzu GC/MS system, model GC-2010Plus, fitted with a mass spectrometer TQ-8040, inlet AOC5000Plus. The column used was a Rtx-5Sil MS (30 m, 0.25 mm ID, 0.25 μm). The oven temperature was kept at 50 °C for 2 min., followed by a ramp at 6 °C min⁻¹ up to 300 °C (held for 15 min). The carrier gas was helium at a constant flow rate of 1.0 mL min⁻¹ (53.5 kPa). The injection volume was 1.0 μL, the split ratio was 1:40, the injector temperature was 280 °C, and the interface temperature was 300 °C. The MS operated at electron ionization mode (70 eV) in a full-scan range (40–550 m/z). The total analysis time was 58.67 min. The retention index of the components that were present in the bio-oils was calculated based on the retention time of the n-alkanes of the petrodiesel sample. The chemical identities of the components present in the bio-oils were determined using NIST Spectrotech 107, NIST 21, and Wiley 8 libraries, and through the retention index database of the NIST.

The development and validation of GC–MS analysis was conducted using the gas chromatograph Shimadzu GCMS TQ 8040 system (Shimadzu, Kyoto, Japan) coupled with the mass spectrometer QP-2010 Ultra (Shimadzu; EI source at 230 °C with 70 eV; scanning 29–500 m/z at 3.3 Hz), an autosampler for static headspace analysis (AOC 5000 plus, Shimadzu, Kyoto, Japan), and a capillary column HP-INNOWAX (30 m × 0.25 mm i.d., 0.25 µm film thickness). The carrier gas was helium of 99.99% purity, flowing at a constant rate of 1.5 mL/min. The temperature graduate program of the column was programmed to have several gradual ramps: (a) from 80 to 140 °C at a rate of 10 °C/min; (b) from 140 to 280 °C at a rate of 20 °C/min; (c) at this point, the GC oven was held at 280 °C for 10 min. The injector heater’s temperature was set to 280 °C. The splitless mode was 1:40 during the analysis. The MS data were obtained by electron impact ionization and used for comparing with the NIST-2017 (National Institute of Standards and Technology, Gaithersburg, MD, USA) and Wiley-08 (Wiley, New York, NY, USA) databases. The MS transfer line and ion source were at 230 °C. The injected volume of sample was 1 µL. The results of phytoconstituent profiles after GC–MS analysis were compared using Adams libraries [44 ,60 ,61 (link)]. All analyses were carried out in triplicate for statistical data processing.

The analysis was performed by head-space gas chromatography/mass spectrometry (HS-GC/MS) with a Shimadzu, mod. 2010 Plus, equipped with a MS detector QP2010 Ultra and an autosampler Shimadzu AOC 5000 Plus. Head space conditions were as follows: temperature 80 °C, time 60 min, injection volume 500 μL. A capillary column Agilent HP5-ms (30 m length, 0.25 mm inner diameter, 0.25 μm film thickness) was used for the separation. Other analytical conditions were as follows: carrier gas Helium at 1 mL/min; incubation temperature 80 °C; incubation time 60 min; splitless injector temperature 200 °C; temperature program hold 40 °C for 3 min—from 40 °C to 260 °C at 40 °C/min; injection volume 500 μL; transfer line temperature 280 °C; source temperature 200 °C; E 70 eV; SIM acquisition mode. Target ions were m/z 32 methyl alcohol (qualifier ion 31), m/z 31 ethyl alcohol (qualifier ion 45), and m/z 31 for 1-propanol (internal standard). The results were expressed in mg/kg.

After sample preparation, the vials were shaken for 30 min at 120 °C in a heated autosampler for static headspace analysis (AOC 5000 plus, Shimadzu, Kyoto, Japan). From the headspace, 2 mL were automatically injected into one of the two injection ports (each at 150 °C; split: 1:10) of a GC-2010 Plus gas chromatograph (Shimadzu) using two separate flowlines with similar columns (HP-5 MS UI 30 m × 0.25 mm × 0.5 µm, Agilent, Santa Clara, CA, USA), running a constant flowrate of 35 cm/s helium and a custom temperature ramp (held at 50 °C for 4 min; with 5 °C/min to 150 °C; with 10 °C/min to 200 °C, held up to a total measurement time of 35 min).
Detection was performed on either the manufacturer-improved ion mobility spectrometer with shorter drift tube and improved ionization area (G.A.S., Dortmund, Germany; drift tube: 15.2 × 53 mm; temperature: 80 °C; ³H-source; 150 mL/min nitrogen as drift gas; field strength: 500 V/cm) or the mass spectrometer QP-2010 Ultra (Shimadzu; EI source at 200 °C with 70 eV; scanning 32–300 m/z at 3.3 Hz).

Four grams of tea leaves were placed in 200 mL of hot distilled water (98°C) and brewed for 5 min. Then, 5 mL of the filtered tea infusion and 1 g of NaCl were placed into 10 mL headspace vials with Teflon‐lined silicon septa (Chromacol, Fisher Scientific). SPME was used to extract volatiles and volatiles were analysed by injection into the GC‐MS using an AOC‐5000 Plus (Shimadzu Scientific, Columbia, MD) SPME auto‐sampler. Samples were equilibrated for 2 min prior to extraction. A DVM/Carboxen/PDMS SPME fiber (2 cm 50/30 um) (Supelco, Bellefonte, PA) was exposed to the headspace above the tea extract in glass vials for 30 min at 40°C with an agitation speed of 250 rpm.

Quantitative analysis of phytocannabinoids was performed using the Shimadzu GC-MS QP2010 system (Shimadzu, Japan). A 30 m long Rxi-5ms (Restek, Bellefonte, PA, USA) column was used for cannabinoids separation. Column thickness—0.25 µm; inner diameter—0.25 µm. Helium was used as the carrier gas. Gas chromatograph conditions: initial column temperature of 110 °C maintained for 2 min, then raised to 190 °C at a rate of 10 °C/min and maintained for 10 min; at a rate of 10 °C/min, the temperature was raised to 280 °C and held for 10 min. The total analysis time for one sample was 39 min. The temperature of the injector was 250 °C, the samples were inserted using an autoinjector (AOC-5000 Plus, Shimadzu, Japan), and the injection was performed by the split 1:10 method. An injection volume of 1 µL was used. The following mass spectrometer conditions were set: ion source temperature: 200 °C, interface temperature: 280 °C, solvent exit time: 2.5 min, and sample ionization energy: 70 eV. Scan speed: 1666; scan interval: start 35.00 m/z, end: 500.00 m/z. The obtained sample chromatograms were analyzed using GCMS solution (Shimadzu, Japan) software. The compounds were identified according to the mass-to-charge ratio by comparing the mass spectra of standard and identified compounds. The quantitative analysis was performed using the external standard method.

To evaluate the specific adsorption of the adsorbent, we used gas chromatography–mass spectrometry (GC-MS) with a solid-phase microextraction (SPME) fiber auto-sampler [16 (link)], as described below.

The adsorbents were placed in a sealed chamber and exposed to odorant gases (Figure 4). The odorants were volatilized at 50 °C in a permeator (PD-1B, GASTEC, Ayase, Japan) or a glass desiccator, and then left in the chamber for 1 h under gas flow at 0.5 L/min.

The adsorbents were transferred to screw tube vials and were introduced into the SPME auto-sampler (AOC5000 plus, Shimadzu, Japan) with an SPME fiber (23-gauge, 50/30 µm, DVB/CAR/PDMS, SPELCO, Bellefonte, PA, USA). The samples were then heated from 40 to 240 °C to desorb the odor molecules from the adsorbents. Finally, the amounts of the detached gases were determined using GC-MS (GCMS-QP2010, Shimadzu, Kyoto, Japan). This method is referred to below as the “GC-MS/SPME method”.