Volatile compounds from Calypogeia azurea were extracted by the headspace solid phase microextraction technique. Fused silica fibres coated with divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) were used. A 2-cm long fibre covered with a 50/30 µm thick film was used. Before analysis, the fibres were conditioned for 1 h at 270 °C, according to the supplier’s instructions. Then, 5 mg of clean and dried plant material was placed in a 1.7 mL vial hermetically closed with a Teflon/silicone septum and heated at 50 °C. The extraction of the compounds was followed at 50 °C for 60 min. Fibre analyte desorption was carried out in the injection port of the gas chromatograph at 250 °C for 10 min. Sorption and desorption operations were performed using the TriPlus RSH autosampler (Thermo Scientific, Waltham, MA, USA).
Triplus rsh autosampler
Manufactured by Thermo Fisher Scientific
Sourced in United States, Germany
The TriPlus RSH autosampler is a versatile instrument designed for automated sample handling and preparation. It is used to introduce liquid, solid, and headspace samples into gas chromatography (GC) or liquid chromatography (LC) systems, enabling efficient and reproducible sample analysis.
Automatically generated - may contain errors
Lab products found in correlation
Trace 1310 gas chromatograph, by Thermo Fisher Scientific (8 mentions)
Trace 1310 gc, by Thermo Fisher Scientific (6 mentions)
Isq single quadrupole mass spectrometer, by Thermo Fisher Scientific (3 mentions)
Db 5ms, by Agilent Technologies (3 mentions)
Tracefinder software, by Thermo Fisher Scientific (2 mentions)
Trace 1300 gc system, by Thermo Fisher Scientific (2 mentions)
Zb wax column, by Thermo Fisher Scientific (2 mentions)
Dvb carboxen pdms, by Merck Group (2 mentions)
Trace 1300 gc, by Thermo Fisher Scientific (2 mentions)
Isq lt single quadrupole mass spectrometer, by Thermo Fisher Scientific (2 mentions)
Q exactive orbitrap, by Thermo Fisher Scientific (2 mentions)
Trace gc ultra, by Thermo Fisher Scientific (2 mentions)
Trace 1300 gas chromatograph, by Thermo Fisher Scientific (2 mentions)
Conflo 4, by Thermo Fisher Scientific (2 mentions)
Trace 1300, by Thermo Fisher Scientific (2 mentions)
Tsq 9000 triple quadrupole mass spectrometer, by Thermo Fisher Scientific (2 mentions)
Trace 1310, by Thermo Fisher Scientific (2 mentions)
Tsq 8000 mass spectrometer, by Thermo Fisher Scientific (2 mentions)
Rtx 624 column, by Restek (1 mentions)
Tsq 8000, by Thermo Fisher Scientific (1 mentions)
43 protocols using triplus rsh autosampler
1
Headspace SPME of Calypogeia azurea
2
Measuring Residual DCM in Microparticles
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The residual dichloromethane in DPH-loaded microparticles was measured using the headspace technique with a TRACE1310 gas chromatograph (GC; Thermo Fisher Scientific, Waltham, MA, USA) equipped with a TriPlus RSH autosampler and a TSQ9000 mass spectrometer (Thermo Fisher Scientific, USA). The sample was placed in a vial and heated before being injected into Rtx-624 column (30 m × 0.32 mm, 1.80 m; Restek Corporation, Bellefonte, PA, USA). The GC oven was initially set at 35 °C for 10 min, then increased to 200 °C for 2 min at a ramp rate of 10 °C/min.
3
GC-MS/MS Analysis of Phthalates
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All the phthalates determination was performed using a GC-MS/MS system (Thermo Fisher Scientific, Waltham, MA, USA), a Trace GC 1310 gas chromatograph, a TriPlus RSH Autosampler and TSQ 8000 mass spectrometer (Thermo, Waltham, MA, USA) and controlled by a computer running TraceFinder software. A DB5-MS (30 m × 0.25 mm × 0.25 µm) gas chromatography column from Agilent (Santa Clara, CA, USA) was used to separate phthalates. Oven temperature was set initially at 100 °C (hold for 1 min), then increased to 280 °C at 10 °C/min and to 310 °C at 5 °C/min. At 310 °C, temperature was maintained for 5 min. Helium was used as a carrier gas in a constant flow of 1 mL/min and the injection volume was 1 µL with an autosampler in splitless mode. The total of analysis time was 20 min. Solvent delay was 1 min. The GC was interfaced by a heated transfer liner (310 °C) to the mass spectrometer in electron ionization mode with an electron energy of 70 eV. Inlet temperature was 290 °C and inject volume was 1 µL. The criteria for the identification of phthalates were based on both the same retention times as the standard within ±2% and correctly relative abundance of two characteristic ions within ±15%. Data processing was done by TraceFinder software from Thermo Fisher Scientific. Identifying and quantifying ions, retention time, and collision energy are listed in Table S1 .
4
Gas Chromatographic Analysis of Fermentation Samples
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Fermentation samples with a volume of 2 ml were analyzed in 15-ml vials with a Thermoscience Trace gas chromatograph equipped with a ResTek Stabilowax polyethylene glycol column with a 0.25-µm diameter. Split injection (1:25), with a resting flow rate of 2 ml/min of He, was performed after 10 min of equilibration at 60°C with a Thermoscience TriPlus RSH autosampler. The oven was kept at 40°C for 2 min, heated to 240°C with a ramping of 15°C/min, and kept at 240°C for 2 min. The detection was carried out with a flame ionization detector (FID), using 20 ml/min of N2, 350 ml/min high-grade compressed air, and 30 ml/min H2 provided from a VWR H2 generator. For the industrial strains, quantification was done under identical chromatography conditions, except that detection was performed with a Thermo Scientific ISQ single quadrupole mass spectrometer. Concentrated standards were kept at −20°C in gas chromatography (GC)-grade absolute ethanol and brought to the final concentration in 5% ethanol in volumetric dilutions, except for wine and saké fermentations, for which 15% ethanol was used in the standards. Fermentation samples were kept at 4°C prior to analysis.
5
Volatile Profiling of Snack Samples
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VSOPs of SDEMs were analyzed using HS-SPME-GC-MS as described by Damerau et al. [41 (link)]. 0.5 g ± 0.005 g of SDEM, 1 g ± 0.01 g of the crushed cookie models, and 1 g ± 0.01 g of finely chopped chocolate models were weighed in triplicate in 20 mL headspace vials and flushed with nitrogen. Volatiles were extracted using HS-SPME using TriPlus RSH autosampler (Thermo Scientific, Reinach, Switzerland) equipped with a DVB/CAR/PDMS-fiber (50/30 μm film thickness; Supelco, Bellefonte, PA, USA). Extraction conditions: agitation speed 250 rpm, incubation 50 °C for 20 min, extraction 50 °C for 30 min, and desorption 240 °C for 6 min. Extracted volatiles were analyzed with TRACE 1310 GC (Thermo Scientific Reinach, Switzerland) equipped with a SPB®-624 capillary column (60 m × 0.25 mm × 1.4 μm, Supelco, Bellefonte, PA, USA) and coupled with an ISQ 7000 MS detector (Thermo Scientific, Reinach, Switzerland). GC-MS conditions: helium flow 1.4 mL/min; oven at 40 °C held 6 min, 5 °C/min to 220 °C and held for 10 min; EI mode 70 eV and scan range 40 to 300 amu. Compounds were identified by the NIST MS Search library (version 2.3. National Institute of Standards and Technology, Gaithersburg, MD, USA) and by comparing retention times and MS spectra of standards.
6
Residual Solvents Analysis by GC-FID
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Samples were analyzed for residual solvents using Thermo Trace 1,300 gas chromatography with flame ionization detection and TriPlus RSH Autosampler and processed with Chromeleon 7.2 software (Thermo Scientific). Supplementary Table S3 shows the parameters used in the residual solvents analysis by gas chromatography.
7
Gas Chromatography-Mass Spectrometry Protocol
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Chemical analyses were performed with a TRACE 1310 gas chromatograph (GC), interfaced to an ISQ single quadruple mass spectrometer (MS) (GC-MS, Thermo Scientific, Waltham, MA, USA), and the system was controlled by the Xcalibur 2.2 software. The GC oven was fit with an HP-5 MS UI capillary column (30 m length × 0.32 mm inner diameter × 0.25 μm film thickness, Agilent Technologies, Santa Clara, CA, USA). Sample injection was performed in splitless mode with helium as the carrier gas at a constant flow of 1 ml min−1. Hexane samples (1 μl) were injected by a TriPlus RSH autosampler (Thermo) and SPME samples were manually injected by inserting the fibers into the GC inlet. Specifically for SPME samples, a narrow-bore glass inlet liner (0.75 mm inner diameter) was used to desorb the loaded SPME fibers. The inlet temperature was maintained at 270°C for 65 μm PDMS/DVB, 280°C for 85 μm PA and 100 μm PDMS, 310°C for 85 μm CAR/PDMS, and 320°C for 7 μm PDMS and hexane samples. The GC running of the column oven was programmed from 60°C for 2 min, then ramped at 30°C min−1 to 200°C (0 min hold) and ramped at 5°C min−1 to 320°C with a 10 min hold. The transfer line was set at 280°C and the mass spectrometer was operated in EI mode with a 70 eV ionization energy. Scanning was recorded from 45 to 650 atomic mass units, at a rate of 5 scans/s.
8
Lipid Extraction and Fatty Acid Analysis
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Lipids were extracted using hexane:isopropanol [39 (link)]. A powdered sample of tissue (∼50 mg) was extracted twice into 3.6 mL of hexane/2-propanol (3:2 v/v) with BHT (50 μM; Sigma-Aldrich, St. Louis, MO, USA) added to limit lipid peroxidation. Samples were homogenized using a PRO200 Bio-Gen Series homogenizer (PRO Scientific Inc., Oxford, CT, USA) and then centrifuged at 2000× g for 10 min. The organic phase was removed, dried under nitrogen, and dissolved in 1 mL of hexane/2-propanol (3:2 v/v) containing 5% water and 50 μM BHT and stored at −80 °C under nitrogen. The FA content of the organic extract was determined by fatty acid methyl ester (FAME) analysis using a Thermo Trace-1310 equipped with a TriPlus RSH Autosampler, (Thermo Fisher Scientific, Waltham, MA, USA) and a Supelco SP-2560 capillary column (75 m, 0.18 mm ID, 0.14 µm film thickness) as previously described [38 (link)]. Fatty acid methyl esters were prepared with the use of acetyl chloride [38 (link)].
9
Volatile Flavor and Lipid Oxidation in Potato Crisps
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The volatile flavour compounds associated with the cheese & onion seasoned potato crisps and the development of lipid oxidation markers in the unsalted potato crisps during accelerated storage were evaluated by the headspace gas analysis performed using solid phase micro-extraction (SPME) and GC-MS. The analysis was performed with an ISQ Single Quadrupole Mass Spectrometer, paired with a TRACE 1300 GC system, equipped with a ZB-WAX column (30 m × 0.25 mm I.D. × 1μm film thickness) and a TriPlus RSH autosampler (Thermo-Fisher Scientific, Waltham, MA, USA). A fused silica fibre coated with a 50/30 μm layer of divinylbenzene–carboxen–polydimethylsiloxane (DVB/CARBOXEN/PDMS; Supelco) was used to analyse headspace samples. The fibre was exposed to the headspace for a total extraction time of 20 min at 70 °C. After extraction, the fibre was immediately thermally desorbed at 250 °C for 4 min. The oven temperature was as follows: 40 °C for 2 min, then to 240 °C at 6 °C min–1, held for 5 min. MS was operated in the electron impact (EI) ionisation mode at 70 eV and data acquisition was achieved at a scan rate of 0.20 s–1 over an m/z range of 35–300. The peak area was processed with Xcalibur Software and identification of aroma compounds using NIST library software (NIST/EPA/NIH Mass Spectral Library, version 2.0, Faircom Corporation, U.S.).
10
Quantitative Analysis of Plant Volatiles
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For dry plant tissue, the sample was
homogenized using a commercial coffee grinder. Samples and standards
were weighed on a VWR-164AC analytical balance (VWR) and analyzed
using a TriPlus 500 GC Headspace Autosampler and a TRACE 1300 GC coupled
with an ISQ 7000 Single Quadrupole MS System (Thermo Fisher).
Where cross-validation was required, samples were also analyzed using
a TriPlus RSH Autosampler, TRACE 1310 GC, and a TSQ 9000 Triple Quadrupole
GC–MS/MS system equipped with an advanced electron ionization
(AEI) source (Thermo Fisher).
homogenized using a commercial coffee grinder. Samples and standards
were weighed on a VWR-164AC analytical balance (VWR) and analyzed
using a TriPlus 500 GC Headspace Autosampler and a TRACE 1300 GC coupled
with an ISQ 7000 Single Quadrupole MS System (Thermo Fisher).
Where cross-validation was required, samples were also analyzed using
a TriPlus RSH Autosampler, TRACE 1310 GC, and a TSQ 9000 Triple Quadrupole
GC–MS/MS system equipped with an advanced electron ionization
(AEI) source (Thermo Fisher).
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