Samples (5000 ll) and 4975 ll pure water (Millipore, Brazil) were poured into 20 ml glass sample vials. NaCl (3 g) and 25 ll of a 25 ng ll -1 methanolic (R)-2-octanol solution, internal standard, were added to each sample. Vials were sealed with a Teflon-faced septum cap and mixed on a magnetic stirrer (IKA, USA) at 1100 rpm. Samples were pre-conditioned at the extraction temperature (40 °C) for 15 min. Polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibers (65 lm; Supelco, USA) were used for HS-SPME. Before use, the fibers were conditioned according to the manufacturer's instructions. After pre-conditioning of the sample, SPME fibers (2 cm) were exposed to the headspace for 15 min at controlled temperature (40 °C) during the extraction process, and the fibers were inserted immediately into the GC injector port (230 °C) for 20 min for thermal desorption of the volatile compounds (Massera et al. 2012) .
Pdms dvb fiber
Manufactured by Merck Group
Sourced in United States
The PDMS/DVB fiber is a lab equipment product used for solid-phase microextraction (SPME) applications. It consists of a polydimethylsiloxane (PDMS) coating with a divinylbenzene (DVB) sorbent layer. The fiber is designed to adsorb a wide range of analytes, making it suitable for various sample preparation techniques in analytical chemistry.
Automatically generated - may contain errors
Lab products found in correlation
Formic acid, by Thermo Fisher Scientific (3 mentions)
Pure water, by Merck Group (1 mentions)
Gc ms, by Thermo Fisher Scientific (1 mentions)
Trace gc ultra, by Thermo Fisher Scientific (1 mentions)
Db 5ms fused silica capillary column, by Agilent Technologies (1 mentions)
Db 1301 column, by Agilent Technologies (1 mentions)
Isopropanol, by Thermo Fisher Scientific (1 mentions)
Mwcnt, by Merck Group (1 mentions)
2 4 dichlorophenol 2 4 dcp, by Sinopharm (1 mentions)
Milli q water purification system, by Merck Group (1 mentions)
Phenol, by Sinopharm (1 mentions)
Agilent 7890b, by Agilent Technologies (1 mentions)
Agilent 5977a, by Agilent Technologies (1 mentions)
Hp 5ms, by Agilent Technologies (1 mentions)
Combi pal autosampler, by Agilent Technologies (1 mentions)
Dvb car pdms fiber, by Merck Group (1 mentions)
11 protocols using pdms dvb fiber
1
Headspace Solid-Phase Microextraction of Volatile Compounds
2
Headspace Solid-Phase Microextraction of Aroma Compounds
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A manual fiber holder and 65 μm polydimethylsiloxane-divinylbenzene (PDMS/DVB) fibers (length = 1 cm), supplied by Supelco (Bellefonte, PA, USA), were employed in this study. Fiber was conditioned before use by inserting into the GC injector port at 250 °C during 30 min, following the manufacturer recommendations. A magnetic stirrer equipped with electronic contact thermometer (IKA®-Werke GmbH & Co. KG, Germany) was used to favor the volatilization of aroma-related compounds into the headspace.
The headspace solid phase micro-extraction (HS-SPME) process was carried out by introducing 10 g of fruit puree into a 20 mL glass vial, together with 1 g of sodium chloride and 40 µL of the IS solution at 1000 mg L−1. The vial was crimped with a polytetrafluoroethylene (PTFE)-faced septum, then immersed into a water bath at 65 °C, and magnetically stirred during 30 min for temperature equilibration. Afterwards, headspace sampling was performed for 20 min at 65 °C, stirring the solution at 800 rpm. Finally, the fiber was withdrawn from the vial and the SPME device was transferred to the GC injection port, where thermal desorption of the analytes was carried out at 240 °C for 5 min.
The headspace solid phase micro-extraction (HS-SPME) process was carried out by introducing 10 g of fruit puree into a 20 mL glass vial, together with 1 g of sodium chloride and 40 µL of the IS solution at 1000 mg L−1. The vial was crimped with a polytetrafluoroethylene (PTFE)-faced septum, then immersed into a water bath at 65 °C, and magnetically stirred during 30 min for temperature equilibration. Afterwards, headspace sampling was performed for 20 min at 65 °C, stirring the solution at 800 rpm. Finally, the fiber was withdrawn from the vial and the SPME device was transferred to the GC injection port, where thermal desorption of the analytes was carried out at 240 °C for 5 min.
3
Profiling Volatile Compounds of Male and Female Butterflies
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The volatiles emitted from eight males and eight females were sampled using the solid-phase microextraction (SPME) technique and analyzed by gas chromatography and mass spectrometry (GC-MS, Thermo Fisher Scientific, Bellefonte, USA). To collect the odor emitted by males and females, we used a conical flask (height: 15 cm, diameter: 3 cm, V: 300 ml) with one small opening and one SPME fiber holder placed in the opening. The sample time was 1 h for the fiber and either eight males or eight females were kept together in the conical flask each time.
Polydimethylsiloxane-divinylbenzene (PDMS/DVB) fibers (65 μm, Supelco, Bellefonte, PA, USA) were used to sample the volatiles from live butterflies31 . The SPME fibers were desorbed before each sampling by heating in a GC injector (250 °C for 10 min) with a He gas flow. Analyses were conducted using a Thermo Fisher TRACE GC ULTRA coupled to a Thermo Fisher ITQ 900 MS. A TR-1MS column (internal diameter: 0.25 mm, film thickness: 0.25 μm, length: 30 m) was used, programmed for 40 °C for 2 min then increased to 120 °C for 2 min (4 °C/min), and then increased to 230 °C for 5 min (5 °C/min) with an injector temperature of 250 °C, and He carrier gas at 69 kPa. Identification of the compounds was made by comparison of retention times and mass spectra with authentic reference samples.
Polydimethylsiloxane-divinylbenzene (PDMS/DVB) fibers (65 μm, Supelco, Bellefonte, PA, USA) were used to sample the volatiles from live butterflies31 . The SPME fibers were desorbed before each sampling by heating in a GC injector (250 °C for 10 min) with a He gas flow. Analyses were conducted using a Thermo Fisher TRACE GC ULTRA coupled to a Thermo Fisher ITQ 900 MS. A TR-1MS column (internal diameter: 0.25 mm, film thickness: 0.25 μm, length: 30 m) was used, programmed for 40 °C for 2 min then increased to 120 °C for 2 min (4 °C/min), and then increased to 230 °C for 5 min (5 °C/min) with an injector temperature of 250 °C, and He carrier gas at 69 kPa. Identification of the compounds was made by comparison of retention times and mass spectra with authentic reference samples.
4
Volatile Compound Analysis of Bamboo Shoots
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The manual SPME device and 65-μm polydimethylsiloxane-divinylbenzene (PDMS/DVB) fiber used in this study were purchased from Supelco Co. (Bellefonte, PA, USA). The PDMS/DVB fiber was conditioned as recommended by the manufacturer prior to the extraction. Fresh B. oldhamii shoots of 3 g in weight was placed a 20-mL vial closed by a polytetrafluoroethene (PTFE)/silicone septum without any solvent, and then heated for 30 min in water baths of 25, 40, 60, and 100 C.
The SPME fiber was then inserted into the vial and adsorbed the volatiles of B. oldhamii shoots in the headspace of the vial. The adsorption time of each extraction was held for 30 min at different temperatures and then desorbed at the gas chromatography (GC) inlet for 5 min at 230 C. Similarly, the samples were steamed at 100 C for various durations before SPME extraction for further analysis.
The SPME fiber was then inserted into the vial and adsorbed the volatiles of B. oldhamii shoots in the headspace of the vial. The adsorption time of each extraction was held for 30 min at different temperatures and then desorbed at the gas chromatography (GC) inlet for 5 min at 230 C. Similarly, the samples were steamed at 100 C for various durations before SPME extraction for further analysis.
5
Volatile Compounds Profiling of Flowers
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The SPME equipped with a 65 μm PDMS-DVB fiber (Supelco, Bellefonte, PA, USA) was inserted into above vial to collect volatile compounds for 30 mins. The collection temperature in our experiment was 50 °C thus volatile in flowers could be stimulated out better. An empty vial was used as control. After 30 mins, the fiber was inserted into the injection of GC for 3 minutes' sample introduction.
The GC conditions in our experiment were as follows: a GC system (Thermo Fisher Scientific, Waltham, MA, USA) was equipped with a DB-5MS fused silica capillary column (30 m× 0.25 mm × 0.25 μm, Agilent Technologies, Santa Clara, CA, USA). Helium was used as carrier gas with flow rate of 1 mL / min. The original temperature was 50 °C for 2 mins and increasing at 5 °C per min to 200 °C with no hold. Then the temperature increased at 10 °C per min to 220 °C.
The MS conditions in our experiment were as follows: the electron ionization mode of the MS was operated at 70 eV, generating a scan range of 45-450 amu. The ion source and transfer line were 200 °C and 250 °C, respectively.
The GC conditions in our experiment were as follows: a GC system (Thermo Fisher Scientific, Waltham, MA, USA) was equipped with a DB-5MS fused silica capillary column (30 m× 0.25 mm × 0.25 μm, Agilent Technologies, Santa Clara, CA, USA). Helium was used as carrier gas with flow rate of 1 mL / min. The original temperature was 50 °C for 2 mins and increasing at 5 °C per min to 200 °C with no hold. Then the temperature increased at 10 °C per min to 220 °C.
The MS conditions in our experiment were as follows: the electron ionization mode of the MS was operated at 70 eV, generating a scan range of 45-450 amu. The ion source and transfer line were 200 °C and 250 °C, respectively.
6
Quantitative Analysis of Volatile Compounds in Juice Samples
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Concentrations of higher alcohols (isobutyl, isoamyl and amyl alcohol, 1-propanol), esters (ethyl acetate, ethyl lactate), methanol, and acetaldehyde were determined using a head space solid phase microextraction (HS-SPME), followed by gas chromatography. First, 10 mL of the juice sample was mixed with 1 mL of 2-pentanol as an internal standard (20 mg/L). Then, to extract the volatile compounds, a poly dimethylsiloxane/Divinylbenzene (PDMS/DVB) fiber (Supelco, PA, USA) was used. A 1.7 mL sample was placed into a 5 mL headspace vial and 0.49 g of sodium chloride was added. After 5 min of equilibration at 25°C and agitation of 1,200 rpm, the fiber was inserted into the headspace and the solution was swirled in a magnetic stirrer at 12,000 rpm and 60°C for 30 min. The fiber was then transferred to the injector for desorption at 270°C for 15 min. Gas chromatography analysis was performed on a Shimadzu Plus 2010 GC system equipped with a flame ionization detector, using a DB-1301 column (60 m, 0.250 mm, film thickness, 1 μm, Agilent). The oven temperature was programmed at 40°C for 16 min, followed by a gradual increase of temperature at a rate of 5°C/min up to 60°C, and then raised to 260°C at a rate of 70°C/min. The gas carrier was hydrogen at a flow rate of 2.0 mL/min.
7
SPME-GC Headspace Sampling in Vacuum
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The SPME polydimethylsiloxane/divinylbenzene (PDMS/ DVB) fiber with a 65-µm-thick coating was purchased from Supelco (Bellefonte, PA). The fiber was conditioned before the initial use, as recommended by the manufacturer. The HS sampling procedure was as follows: a cap-sealed (silicon/ PTFE lined alumina cap) 22 ml vial containing the sample was kept at 50 °C for 10 min in an aluminum heating block (IKA RCT, Model B). Afterwards, the SPME fiber was exposed to the sample for 30 min at 50 °C. After sampling, the compounds on the fiber were thermally desorbed in the GC injection port. The sample was cheese or standard compounds in water, depending on the experiment.
For the vacuum experiments prior to the analyses the pressure was lowered at room temperature by removing 20 ml of air from the sealed vial using a 30 cc MICRO-MATE interchangeable glass syringe from Popper and Sons, Inc. (New York, USA). Unlike at ambient pressure, SPME was used in vacuum sampling Mininert closures, as described in [10] . Because of the nature of the matrix for analyses, cheese was closed in the vial, capped and then air was evacuated with a syringe. Usually for liquid matrices, first the air was evacuated from the vial, then the (liquid) sample was introduced [8] .
For the vacuum experiments prior to the analyses the pressure was lowered at room temperature by removing 20 ml of air from the sealed vial using a 30 cc MICRO-MATE interchangeable glass syringe from Popper and Sons, Inc. (New York, USA). Unlike at ambient pressure, SPME was used in vacuum sampling Mininert closures, as described in [10] . Because of the nature of the matrix for analyses, cheese was closed in the vial, capped and then air was evacuated with a syringe. Usually for liquid matrices, first the air was evacuated from the vial, then the (liquid) sample was introduced [8] .
8
Headspace SPME Analysis of Volatile Flavor Compounds
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SPME fibre (65 μm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber, Supelco, Bellefonte, PA, USA) was used for flavor extraction. The fiber was previously conditioned at 250 °C for 1 h before each use. Five grams of the weighed oil sample was placed into a 20 mL glass vial which was sealed with an aluminum cover and a Teflon septum. The samples were heated at 50 °C for 20 min in a thermostatic bath with a magnetic stirrer and extracted for 40 min using an auto SPME holder containing fiber. Subsequently, the fiber was injected into the gas chromatography-mass spectrometry (GC-MS) system (Shimazu QP2010 SE, Kyoto, Japan). The volatiles absorbed by the fiber were thermally desorbed in the hot injection port of the GC for 2 min at 250 °C.
9
Phenolic Compounds Analysis Protocol
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Phenol, p-nitroPhenol (4-NP), o-nitroPhenol (2-NP), 2, 4-dimethylPhenol (2,4-DMP), and 2,4-dichloroPhenol (2,4-DCP) standards were purchased from Sinopharm Chemical Reagent Co., Ltd. (Shanghai, China). Hydrogen nitrate (AR grade, purity 65–68%) and sulfuric acid were purchased from Guangzhou Chemical Reagents (Guangzhou, China). HPLC-grade acetonitrile (ACN), methanol, isopropanol, and formic acid were from Thermo Fisher Scientific Co. (Waltham, MA). Fused-silica fibers (120 µm i.d.) were obtained from Ruifeng Chromatographic Device Co. Ltd (Yongnian, China). MWCNTs (20–30 nm, purity > 98% mass fraction) were purchased from Sigma–Aldrich (St. Louis, MO). SPME hand shank and PDMS/DVB fiber (1 cm length, 65 µm thick, Supelco, USA) were purchased from Sigma-Aldrich Co., Ltd. (Shanghai, China). Acrylic ester was obtained from Guangzhou Chemical Reagents. Sodium deoxycholate (NaDC) was purchased from Aladdin Chemistry (Shanghai, China). Ultrapure water was prepared with a Milli-Q water purification system (Millipore, Bedford, MA). All other chemicals were of analytical grade.
10
Volatile Organic Compounds Analysis of Turbot
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The VOCs of turbot samples were determined using the method portrayed by Li et al. [38 (link)]. Thereby, 3 g minced muscle samples and 6 mL saturated NaCl solution were transferred into a 20-mL sample vial. A 65 μm PDMS/DVB fiber (Supelco, PA, USA) was exposed to the headspace of the vial at 50 °C for 25 min. After extraction, the fiber was directly desorbed into the injection port of the GC at 250 °C. The analytes were determined by GC/MS (GC, Agilent 7890B; MS, Agilent 5977A, Agilent, CA, USA) equipped with a methyl polysiloxane capillary column (HP-5MS, Agilent; 30 m × 0.25 mm × 0.25 μm film thickness). The carrier gas was helium at 1.0 mL/min. The GC column temperature procedure was set as follows: kept at 40 °C for 10 min, increased to 240 °C at 5 °C/min, increased to 280 °C at 20 °C/min, and held for 8 min. The MS operated in electron impact (EI) mode with EI energy of 70 eV; and collected data at a rate of 0.7 scans/s over a range of m/z 40–650. The VOCs were tentatively identified by the comparison of actual mass spectra with the published authentic spectra database in the GC/MS libraries (NIST2011), and the compounds with MS match index over 800 were reported.
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