FKBT and 1Y-KBT (produced in 2020 and 2019, respectively) were acquired from Anhui Guorun Tea Industrial Co., Ltd. (Chizhou City, Anhui, China). The 1Y-KBT sample was stored in a cabin that could keep a relatively stable storage environment. After their acquisition, the samples were stored in a clean, odorless environment at −20 °C. The distilled water used in the experiments was purchased from Watsons Water Company, Inc. (Guangzhou, China). Chromatographically pure methyl tert-butyl ether (MTBE) and pentane were purchased from Aladdin (Shanghai, China) and redistilled before use; 2-octanol and ethyl decanoate (99.5% and 99% pure) were also obtained from Aladdin. n-Alkanes (C5–C40; Sigma-Aldrich, St. Louis, MO, USA) were employed to assist in identifying volatiles by enabling the calculation of retention indices. A solid-phase extraction (SPE) cartridge (LC-Si, 500 mg/6 mL) and a solid-phase microextraction (SPME) needle (50/30 μm DVB/Carboxen/PDMS) were purchased from Supelco (St. Louis, MO, USA). All reference aroma compounds were chromatographically pure and commercially obtained, and the actual purities were confirmed through GC-MS.
Dvb carboxen pdms
Manufactured by Merck Group
Sourced in United States
The DVB/Carboxen/PDMS is a type of lab equipment that functions as a sorbent material. It is composed of a combination of divinylbenzene (DVB), Carboxen, and polydimethylsiloxane (PDMS). This sorbent material is designed to facilitate the extraction and concentration of a wide range of analytes during sample preparation processes.
Automatically generated - may contain errors
Lab products found in correlation
1 2 dichlorobenzene solution, by Merck Group (3 mentions)
Zb wax column, by Thermo Fisher Scientific (2 mentions)
Triplus rsh autosampler, by Thermo Fisher Scientific (2 mentions)
Model 6890, by Agilent Technologies (1 mentions)
Hp 5 column, by Agilent Technologies (1 mentions)
Agilent 7890 gc, by Agilent Technologies (1 mentions)
5975 ms detector, by Agilent Technologies (1 mentions)
Masshunter workstation software, by Agilent Technologies (1 mentions)
Trace gcms, by Thermo Fisher Scientific (1 mentions)
Cp wax 52 capillary column, by Agilent Technologies (1 mentions)
Trace 1300 gc system, by Thermo Fisher Scientific (1 mentions)
Isq single quadrupole mass spectrometer, by Thermo Fisher Scientific (1 mentions)
Gc ms 4000, by Agilent Technologies (1 mentions)
Db waxetr, by Agilent Technologies (1 mentions)
Gcms qp2010 se, by Shimadzu (1 mentions)
Mps2 autosampler, by Gerstel (1 mentions)
Agilent 6890 gc, by Agilent Technologies (1 mentions)
5973 n ms detector, by Agilent Technologies (1 mentions)
Agilent 7890b, by Agilent Technologies (1 mentions)
National institute of standards technology mass spectral database, by Agilent Technologies (1 mentions)
17 protocols using dvb carboxen pdms
1
Identification of Volatile Compounds in Tea
2
Volatile Compound Extraction and Analysis
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One gram mince was put into a 15 ml sample bottle (Supelco), then added 2 ml distilled water and 0.5 g NaCl, followed by SPME immediately. The SPME fiber used was divinylbenzene/Carboxen/poly(dimethyl‐siloxane) (DVB/Carboxen/PDMS) (50/30 μm, 2 cm) (Supelco), exposure time was 60 min, and temperature was 25°C (Fu et al., 2009 ).
GC–MS was conducted in a gas chromatography system equipped with a SH‐Rtx‐5 SIL MS capillary column and an electron ionization ion source operated at 70 eV. Temperature programming was applied from 35°C to 220°C at a rate of 10°C/min. The volatile compounds (hexanal, octanal, nonanal, decenal, 1‐hexanol, 1‐octen‐3‐ol, and 2‐ethyl‐1‐hexanol) were quantified using external standard methods (the standards were purchased from Sigma). The results are the means of three measurements (standard deviation <8%).
GC–MS was conducted in a gas chromatography system equipped with a SH‐Rtx‐5 SIL MS capillary column and an electron ionization ion source operated at 70 eV. Temperature programming was applied from 35°C to 220°C at a rate of 10°C/min. The volatile compounds (hexanal, octanal, nonanal, decenal, 1‐hexanol, 1‐octen‐3‐ol, and 2‐ethyl‐1‐hexanol) were quantified using external standard methods (the standards were purchased from Sigma). The results are the means of three measurements (standard deviation <8%).
3
SPME-GC-MS Analysis of Volatile Compounds
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The solid-phase micro-extraction-gas chromatography-mass spectrometry (SPME-GC-MS) analysis was conducted following our previous studies [40 (link),41 (link)] with some modifications. Volatiles were extracted using an SPME fiber (50/30 μm DVB/Carboxen/PDMS; Supelco, Bellefonte, PA, USA). The SPME fiber was put into the headspace vial, and 1 cm of it was exposed from the headspace for 40 min at 50 °C. After extraction, the fiber was inserted into the injector of a GC-MS (Model 6890; Agilent, Santa Clara, CA, USA) to desorb the adsorbed substances for 5 min at 250 °C. At the same time, the instrument data acquisition was performed.
Gas chromatography was performed using the HP-5 column (50 m × 0.32 mm × 1.05 μm, J&W Scientific, Agilent, Santa Clara, CA, USA) with helium as the carrier gas (37 kPa). The column temperature was set at 40 °C for 2 min, then increased to 250 °C at the rate of 5 °C min−1, and finally maintained at 250 °C for the next 2 min. The volatile compounds were matched against the NIST08 library (NIST/EPA/NIH, American), and the retention indexes were compared with the standard volatile compounds. A standard peak area vs. concentration curve was prepared from the serial dilutions of the standard and used for sample quantification.
Gas chromatography was performed using the HP-5 column (50 m × 0.32 mm × 1.05 μm, J&W Scientific, Agilent, Santa Clara, CA, USA) with helium as the carrier gas (37 kPa). The column temperature was set at 40 °C for 2 min, then increased to 250 °C at the rate of 5 °C min−1, and finally maintained at 250 °C for the next 2 min. The volatile compounds were matched against the NIST08 library (NIST/EPA/NIH, American), and the retention indexes were compared with the standard volatile compounds. A standard peak area vs. concentration curve was prepared from the serial dilutions of the standard and used for sample quantification.
4
GC-MS analysis of fruit juice volatiles
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Volatiles were analyzed using a headspace–solid-phase microextraction (SPME)–gas chromatography–MS system as previously reported (40 ). Briefly, 6 ml of juice was sealed in 20-ml vials and stored at −20°C until analysis. The juice sample was incubated at 40°C for 30 min, and, then, a 2-cm tri-phase SPME fiber (50/30 μm DVB/Carboxen/ PDMS, Supelco, Bellefonte, PA, USA) was inserted to the headspace to collect and concentrate volatiles for 30 min. The SPME fiber was then inserted into the injector of an Agilent 7890 GC coupled with a 5975 MS detector (Agilent Technologies, Palo Alto, CA, USA) for 15 min at 250°C. The column was a DB-5 [60 m–by–0.25 mm inside diameter, 1.00-μm film thickness, J&W Scientific, Folsom, CA, USA). Mass units were monitored from 30 to 250 mass/charge ratio (m/z) and ionized at 70 eV. Volatile identification and quantification of peak areas were conducted with MassHunter Workstation software (version 10.0; Agilent Technologies). Initial identification was done by mass spectra searches with the NIST library (version 14, match score > 0.9). The identification was then confirmed by comparing the retention indices generated by running standard C6-C17 alkane mixture under the same conditions as the samples with online resources (NIST Chemistry WebBook and Flavornet.org ). Each sample had four replicates.
5
Volatile Aldehydes Determination in Burgers
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The volatile aldehydes were determined on 63 burgers by SPME-GC/MS. Five grams of each sample were put into a 20-mL glass. Headspace conditioning was achieved in 15 min, by keeping the sample in a water bath at 35°C. A SPME fiber (50/30 µm; 2-cm long, DVB/Carboxen/PDMS; Supelco, Bellefonte, PA), conditioned for 30 min at 270°C in a GC injector, was exposed to the headspace for 30 min. Lastly, the sample was injected into a single quadrupole GC/MS apparatus (TRACE GC/MS, Thermo-Finnigan, Waltham, MA) coupled with a Varian CP-WAX-52 capillary column (60 m × 0.32 mm; coating thickness 0.5 μm). The injector was set at 250°C and the complete volatile organic compounds (VOCs ) desorption was achieved in 30 min. The oven GC program temperature was set according to Serra et al. (2009) (link). The temperature of the transfer-line and the ion source was 250°C, while the filament emission current was set at 70 eV. The acquisition was performed in full scan mode (TIC) using a mass range from 35 to 270 m/z (1.6 amu/s).
6
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.).
7
GC-MS Analysis of Sweet Potato Crisps Aroma
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The volatile aroma compounds associated with the sweet potato crisps were measured using gas phase solid phase micro-extraction (SPME) with GC-MS. The method was derived from ref. 11 (link) as detailed below. The analysis was completed using an ISQ Single Quadrupole Mass Spectrometer, TRACE 1300 GC, with a TriPlus RSH autosampler (Thermo-Fisher Scientific, Waltham, MA, USA) and a ZB-WAX column (30 m × 0.25 mm I.D. × 1 μm film thickness). The SPME fibre was coated with a 50/30 μm layer of divinylbenzene–carboxen–polydimethylsiloxane (DVB/CARBOXEN/PDMS; Supelco) for analysis. Fibre exposure time in the headspace was 20 min at 70 °C. Subsequently, the fibre was thermally desorbed immediately for 4 min at 250 °C. The temperature ramp in the GC oven was: 40 °C (2 min), ramping to 240 °C at 6 °C min−1, hold at 240 °C for 5 min.11 (link) MS was operated in 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.).
8
Headspace SPME-GC Analysis of Fermented Milk
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Volatile compounds were collected in an SPME system. For each analysis, 20 mL of fermented milk was placed in a 100-mL gas washing flask with a purge head, and 1 μL of 1,2-dichlorobenzene solution (Sigma-Aldrich, St. Louis, MO) was added as internal standard solution. The final concentration of internal standard solution in each sample was 10 μg/L. Under magnetic stirring (200 rpm), the sample was extracted at 50°C for 1 h (Dan et al., 2017) (link), and an SPME fiber (50/30 μm DVB/Carboxen/PDMS; Supelco, Inc. Bellefonte, PA) was exposed in the headspace. The fiber was then inserted into the injection port of a 7890 B GC (Agilent Technologies Inc., Palo Alto, CA) for 3 min at 270°C to desorb volatile compounds into the GC column.
9
Volatile Profiling of EVOO Cultivars by HS-SPME/GC-MS
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The headspace, solid-phase microextraction followed by gas chromatography mass spectrometry (HS-SPME/GC-MS) technique was used to detect and quantify the volatile compounds in the control and PEF EVOOs of the Carolea, Ottobratica, and Coratina cultivars.
The SPME was carried out holding the vials, with 3 g of EVOO and 50 μL of a standard methanolic solution, at 35°C and then the SPME fiber (a 50/30 μm 1 cm long DVB/Carboxen/PDMS, Stableflex; Supelco, Inc., Bellefonte, PA, USA) was exposed to the vapor phase for 30 min to detect the volatile compounds.
The GC-MS analysis were conducted using a Varian 4000 GC-MS equipped with a 1079 split/splitless injector (Varian). The fused-silica capillary column (DB-Wax-ETR, 50 m, 0.32 mm i.d., 1 μm film thickness; J&W Scientific, Folsom, CA, USA) was operated with helium regulated by an electronic flow controller (EFC) at a constant flow rate (1.7 ml min−1). All the operative conditions was set following the method described by Veneziani et al. (7 (link)) without any modifications. The data of the peak areas were evaluated on the basis of calibration curve of each different compound and expressed in μg kg−1 of EVVO (Figure 3 ).
The SPME was carried out holding the vials, with 3 g of EVOO and 50 μL of a standard methanolic solution, at 35°C and then the SPME fiber (a 50/30 μm 1 cm long DVB/Carboxen/PDMS, Stableflex; Supelco, Inc., Bellefonte, PA, USA) was exposed to the vapor phase for 30 min to detect the volatile compounds.
The GC-MS analysis were conducted using a Varian 4000 GC-MS equipped with a 1079 split/splitless injector (Varian). The fused-silica capillary column (DB-Wax-ETR, 50 m, 0.32 mm i.d., 1 μm film thickness; J&W Scientific, Folsom, CA, USA) was operated with helium regulated by an electronic flow controller (EFC) at a constant flow rate (1.7 ml min−1). All the operative conditions was set following the method described by Veneziani et al. (7 (link)) without any modifications. The data of the peak areas were evaluated on the basis of calibration curve of each different compound and expressed in μg kg−1 of EVVO (
10
SPME Fiber Extraction and Analysis
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Three SPME fibers were used: 85 µm Carboxen-PDMS, 65 µm poly(divinylbenzene)(DVB)-PDMS, and 50/30 µm DVB-Carboxen-PDMS (Supelco, Bellafonte, PA, USA). The samples were equilibrated at 30 °C for 5 min, and the extraction took place for 20 min with agitation at 250 rpm. The injection temperatures for each fiber were 300 °C, 250 °C, and 270 °C, respectively. The samples were analyzed in triplicate.
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