The methodological approach was based on works carried out by Tejedor-Calvo et al. [28 (link)], with some modifications. For that, a fused silica fiber coated with a 50/30 mm layer of divinylbenzene/carboxen/polydimethylsiloxane from Supelco (Barcelona, Spain) was chosen. The samples (2 g of powder material) were placed in a 20 mL glass vial closed with a septum. After the vial was conditioned at 50 °C for 10 min, the fiber was exposed to the headspace of the vial for 20 min.
Divinylbenzene carboxen polydimethylsiloxane
Manufactured by Merck Group
Sourced in United States, Spain
Divinylbenzene/carboxen/polydimethylsiloxane is a solid-phase microextraction (SPME) fiber coating used in gas chromatography. It is designed to effectively extract a wide range of volatile and semi-volatile organic compounds from various sample matrices.
Automatically generated - may contain errors
Lab products found in correlation
Agilent 6850 gc, by Agilent Technologies (1 mentions)
Amber vials, by Merck Group (1 mentions)
5973 network mass selective detector, by Agilent Technologies (1 mentions)
Hp 5ms capillary column, by Agilent Technologies (1 mentions)
Spme fiber, by Merck Group (1 mentions)
Gcms qp2010 se, by Shimadzu (1 mentions)
Isq single quadrupole mass spectrometer, by Thermo Fisher Scientific (1 mentions)
Supelcowax 10 capillary column, by Merck Group (1 mentions)
Lynxeye xe detector, by Bruker (1 mentions)
Nicolet is10 ft ir spectrometer, by Thermo Fisher Scientific (1 mentions)
Jsm 7800f field emission scanning electron microscope, by JEOL (1 mentions)
D8 discover instrument, by Bruker (1 mentions)
Zb 5ms column, by Agilent Technologies (1 mentions)
Agilent 7820 gc with 5975 msd, by Agilent Technologies (1 mentions)
Methanol, by Merck Group (1 mentions)
15 protocols using divinylbenzene carboxen polydimethylsiloxane
1
Headspace SPME Analysis of Powders
2
Headspace SPME Analysis of Durian Volatiles
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SPME was carried out according to Zhang et al. (2007) (link). A total of 50 g of fresh durian pulp and FD durian were homogenized with 100 mL of NaCl solution (0.08 g/mL) and stirred for 1 min. Following this, 12.5 mL homogenates were put into a 22 mL vial with the top cap number 2713 and put into the vial the magnetic stirrer (p × d = 10 mm × 3 mm). Next, 0.5 µL of internal standard (IS) 1,4-dichlorobenzene 0.01% (w/v) was spiked into the sample and the vial was tightly closed. SPME fiber syringe (divinylbenzene-carboxenpolydimethylsiloxane 85 µm, Supelco Inc., PA, USA) was manually inserted to the vial headspace at 30°C for 30 minutes and injected into GC-MS.
3
Aroma Characterization of Vitamin Concentrates
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Headspace SPME, followed by GC-O, was conducted to characterize aroma-active compounds extracted from vitamin concentrates. Ten milliliters of vitamin concentrate was added to 40-mL amber vials (28 × 98 mm; Supelco Inc.) with a stir bar, in duplicate. The vials were heated at 40°C for 30 min with constant stirring. An SPME fiber (divinylbenzene/carboxen/ polydimethylsiloxane; Supelco Inc.) was exposed in each sample at 2 cm for 30 min. The fiber was then injected on an Agilent 6850 GC flame-ionization detector equipped with an olfactometer port (Agilent Technologies Inc.). The GC method used an initial temperature of 40°C for 3 min. The temperature was then increased at a rate of 10°C/min to 150°C, followed by 30°C/min to 200°C, and held for 5 min. Samples were evaluated in duplicate on 2 different columns: polar ZB-WAX (30-m length × 0.25-mm i.d. × 0.25-µm film thickness; Zebron; Phenomenex Inc.) and a nonpolar ZB-5 (30m length × 0.25-mm i.d. × 0.25-µm film thickness; Zebron; Phenomenex Inc.). The flame ionization detector sniffing port was held at a temperature of 300°C, with a helium carrier gas flow of 2 mL/min, and the port was supplied with humidified air at 30 mL/min. Each sample was evaluated on each column by 2 highly experienced sniffers (each with >50 h previous experience with GCO) who recorded retention time, aroma character, and perceived intensity.
4
GC-MS Analysis of Volatile Compounds
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For chemical synthesis, see SI Appendix, SI Materials and Methods . Gas chromatography-mass spectrometry was performed on a 5973 Network Mass Selective Detector linked to a 6890 GC Series Plus+ (Agilent Technologies). The GC was equipped with an HP-5MS capillary column (30 m × 0.25 mm; 0.25-µm film; Agilent Technologies), which was operated with the following programs: 70 °C for 1 min, subsequently increased at a rate of 10 °C/min to 270 °C, and held at this final temperature for 10 min.
Injector was operated at 250 °C in pulsed splitless mode. MS transfer line was set at 280 °C, and the MS quad and MS sources were set at 150 °C and 230 °C, respectively. SPME analysis was done with 50/30 divinylbenzene/carboxen/polydimethylsiloxane (catalog # 57328-U; Supelco). Volatile compounds were collected from the headspace of the samples placed in a closed glass container with a rubber septum on the top. SPME analyses were performed with the oven starting at 35 °C for 5 min, raised to 70 °C at a rate of 2.5 °C/min, then raised at 5 °C/min to 150 °C, and subsequently raised to the final temperature of 250 °C at 10 °C/min. Under these conditions, acetaldehyde peak appeared at 1.48 min followed by ethanol peak at 1.59 min.
Injector was operated at 250 °C in pulsed splitless mode. MS transfer line was set at 280 °C, and the MS quad and MS sources were set at 150 °C and 230 °C, respectively. SPME analysis was done with 50/30 divinylbenzene/carboxen/polydimethylsiloxane (catalog # 57328-U; Supelco). Volatile compounds were collected from the headspace of the samples placed in a closed glass container with a rubber septum on the top. SPME analyses were performed with the oven starting at 35 °C for 5 min, raised to 70 °C at a rate of 2.5 °C/min, then raised at 5 °C/min to 150 °C, and subsequently raised to the final temperature of 250 °C at 10 °C/min. Under these conditions, acetaldehyde peak appeared at 1.48 min followed by ethanol peak at 1.59 min.
5
Volatile Cheese Compounds Analysis
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The samples used for the study of the cheese volatiles were portions of the exterior of the cheeses (approximately 1 cm depth). This part was selected because the results obtained in previous studies carried out in our laboratory with other types of cheese revealed that this part was the richest in volatile components [12 (link),15 (link)]. The samples were chopped and approximately 1 g of the chopped sample was weighed into a 4 mL amber vial screw top (acquired from Supelco, Bellefonte, PA, USA), sealed with a hole cap polytetrafluoroethylene/silicone septum, and stored frozen until its study.
Each vial containing 1 g of the cheese sample was introduced into a water bath maintained at 50 °C; then, the fiber was exposed to the headspace of the sample and was maintained for 60 min. The fiber used was coated with divinylbenzene/carboxen/polydimethylsiloxane (50/30 µm film thickness), and it was acquired from Supelco. The selection of the fiber type and the extraction conditions was based on previous studies carried out in our laboratory [11 (link)]. Each cheese was analysed in duplicate.
Each vial containing 1 g of the cheese sample was introduced into a water bath maintained at 50 °C; then, the fiber was exposed to the headspace of the sample and was maintained for 60 min. The fiber used was coated with divinylbenzene/carboxen/polydimethylsiloxane (50/30 µm film thickness), and it was acquired from Supelco. The selection of the fiber type and the extraction conditions was based on previous studies carried out in our laboratory [11 (link)]. Each cheese was analysed in duplicate.
6
Urinary VOCs Extraction by HS-SPME
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Urine was thawed on ice and centrifuged at 13 000 × g for 10 min. The supernatant was divided into 200 µL within a 2 mL glass vial packed tightly with a magnetic gold seal (PTFE/silicone septum 9 mm diameter × 1 mm thickness, GL Science, Tokyo, Japan), and disinfected at 65 °C for 15 min. Urinary VOCs in vials were extracted by headspace solid-phase microextraction (SPME) methods, in which the fiber was constructed with 2 cm 50/30 µM divinylbenzene/carboxen/polydimethylsiloxane (Supelco, Bellefonte, PA, USA). The SPME was preconditioned at 240 °C for 20 min and inserted into the headspace of the vial, including the urine. Finally, the VOCs in the headspace were extracted using SPME fiber at 45 °C for 60 min from the 18 urine samples (9 patients and 9 controls).
7
Headspace SPME analysis of eggplant oil
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The absolute oil (100 mg) in an eggplant flask (25 mL) was allowed to stand for 5 min at 30℃. A SPME fiber, 50/30 μm divinylbenzene / carboxen / polydimethylsiloxane (1 cm, Supelco, Bellefonte, PA) , was introduced through a septum and adsorbed for 1 min at 30℃. The fiber was desorbed for 1 min at an injection port of GC-MS or chiral GC.
8
Quantification of Tea Indole Compounds
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To assay internal indole, finely powdered tea leaves (200 mg) were extracted for 6 h with CH2Cl2 (700 µl) containing d7-labeled indole as an internal standard. The extracts were dried over anhydrous sodium sulfate. Extracts (1 µl) were subjected to GC-MS analysis. To assay the emission of indole, 10 tea shoots containing one bud and three leaves were placed in a beaker sealed with aluminum foil. Solid-phase microextraction (SPME; divinylbenzene/carboxen/polydimethylsiloxane, Supelco Inc.) was used to collect emission volatiles for 20 min at 25 °C, which were then subjected to GC-MS (GCMS-QP2010 SE, Shimadzu, Kyoto, Japan) analysis using a SUPELCOWAX 10 column (30 m×0.25 mm×0.25 µm, GL Sciences, Tokyo, Japan). The GC-MS temperature program was as follows: initial temperature, 60 °C for 3 min; increased to 240 °C at 4 °C min–1; and maintained at 240 °C for 20 min. Full scan mode (m/z 40–200) was used.
9
Volatile Profiling of Apple Pomace and Beer
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The volatile profiles of apple pomace samples fermented and unstarted, before and after the heating treatment, and beer samples with and without the addition of apple pomace, at time zero and after the maturation time (30 days), were analyzed by HS-SPME/GC-MS technique, following the protocol reported by Ricci et al. (2018) [8 (link)]. Samples of 2 g of apple pomace or 2 mL of beer were used for the analyses, adding 10 µL of an aqueous toluene standard solution (100 µg/mL), useful for the semi-quantification of all detected signals. Head space micro-extraction was performed using a SPME fiber coated with three polymers of different polarity, divinylbenzene–carboxen–polydimethylsiloxane (Supelco, Bellefonte, PA, USA). The analyses were performed on a Thermo Scientific Trace 1300 gas chromatograph coupled to a Thermo Scientific ISQ single quadrupole mass spectrometer equipped with an electronic impact (EI) source (Thermo Fisher Scientific, Waltham, MA, USA), and the separation of analytes was achieved on a SUPELCOWAX 10 capillary column (Supelco, Bellefonte, PA, USA; 30 m × 0.25 mm × 0.25 µm). The characteristic volatiles were identified both by comparing mass spectra with the library (NIST 14) and by calculating their linear retention indices (LRIs).
10
Volatile Compound Analysis by SPME-GC
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Volatile compound analysis was carried out by using an optimized solid phase micro extraction (SPME) technique. A 50/30 μm divinylbenzene/carboxen/polydimethylsiloxane (Supelco, Bellefonte, PA, USA) fiber was selected as the most suited for the purpose. One milliliter of sample, 10 μL of internal standard solution (2-Octanol, 82 ng), and 0.14 g of NaCl were inserted into a 15 mL glass vial and closed with a screw cap with a perforable septum. Samples were heated up to 50 °C and held for 10 min for the equilibration phase, then the fiber was inserted into the vial headspace for 30 min for the adsorption of volatile compounds. Thereafter, volatiles were desorbed by inserting the fiber into the gas chromatograph (GC) injector for 3 min.
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