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9 protocols using 3 heptanone

1

Volatile Compound Identification in Ground Coffee

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For better identification of those volatile compounds that are more odour active, ground coffee (3 g) was placed into GC headspace vials (20 mL, 22.5 mm × 75.5 mm, Sigma-Aldrich, UK). 3-Heptanone was used as internal standard (15 μL, 0.01% 3-Heptanone (Sigma, Saint Louis, USA) in methanol (Laboratory reagent grade, Fisher Scientific, UK)) to calibrate for any instrument drift.
Aroma sampling conditions were conducted according to Liu et al. (2019) (link). For GC-O nasal impact frequency (NIF) analysis, a splitter was fitted to the end of the ZB‐WAX column, and approximately half of the flow was diverted to an ‘odour sniffing port’ via a fused silica capillary passing within a heated transfer line, set at a temperature of 200 °C. Six panellists (four males and two females aged between 24 and 35 years) were used to conduct the GC-O NIF analysis. During each GC run, the panellist placed their nose close to the top of the sniffing port and recorded the time, duration and description of odours perceived (Pollien, Ott, Montigon, Baumgartner, Muñoz-Box, & Chaintreau, 1997 ). As the GC runs were 40 min long, two assessors were used to sniff each chromatogram, swapping over half‐way, to avoid fatigue.
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2

Comprehensive Ketone Characterization Protocol

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The following liquid substances were purchased from Sigma-Aldrich: 2-pentanone (98%), 3-pentanone (99%), 2-hexanone (98%), 3-hexanone (98%), 3-heptanone (analytical standard), 4-heptanone (98%), 2-nonanone (99%), 3-nonanone (99%), 2-decanone (98%), cyclohexanone (99.8%), 3-methyl-2-pentanone (99%), 2-methyl-3-pentanone (97%), 2-methyl-3-hexanone (98%), and 2-methyl-3-heptanone (99%). 2-butanone (99.5%), 2-heptanone (98.5%), and 3-methyl-2-butanone (98.5%) were purchased from Honeywell. 3-octanone (99%) and 3-decanone (97%) were purchased from Acros Organics and SAFC, respectively. These were used with no further purification.
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3

Analytical Standards Acquisition for Research

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Pure chemicals: 1-octanol; 1-octen-3-ol; hexanal; heptanal; octanal; nonanal; 2-decenal, (E); benzaldehyde; hexanoic acid; octanoic acid; dodecanoic acid; benzene, 1,4-dimethoxy; 2-hexen-1-ol, (E); 2-hexen-1-ol, acetate, (E); 3-heptanone, 2-methyl; acetic acid, pentyl ester; acetic acid, hexyl ester; butanoic acid, methyl ester; butanoic acid, ethyl ester; butanoic acid, butyl ester; hexanoic acid, ethyl ester; linalool; γ-dodecalactone and toluene-d8 were purchased from Sigma-Aldrich (Madrid, Spain). The analytical standards n-alkanes mixture (C10–C40) for retention index (RI) assessment determination was supplied by Supelco (St. Louis, USA).
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4

Sweet Potato Crisps Manufacturing Protocol

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Three independent batches of “slightly salted” sweet potato crisps from same sweet potato variety were supplied from Pipers Crisps Ltd (Lincoln, UK), each batch was manufactured independently to ensure true replicates were used throughout. The basic composition of “slightly salted” SPC, fried at 140 °C for 150 s is 573 kcal per 100 g, carbohydrates 39.6% of which sugars are 18.4%, protein 4.6%, dietary fibre 7.6%, fat 45.2% (of which saturated 3.3%) and salt 0.51%, all data relates to a standard 100 g serving. 3-Heptanone used as an internal standard during SPME-GC-MS analysis was supplied by Sigma-Aldrich (UK).
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5

Potato Crisps Flavor Composition

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Unsalted potato crisps and cheese & onion flavour potato crisps were supplied by Pipers Crisps Ltd (Lincoln, UK), where 4 batches (2 batches with N2 gas flushing and 2 batches without gas flushing, from each batch of 6 boxes sized 40 × 40 g) of each product were supplied. Cheese & onion flavour produced using all natural ingredients was supplied by Frutarom (UK). The basic composition of unsalted potato crisps for the 100 g pack is energy 553 Kcal, carbohydrates 56.1% of which sugars are 0.6%, protein 4.9%, fibre 3.8%, fat 33% (of which saturated 3.5%) and salt 0.06%. 3-Heptanone used as an internal standard during SPME-GC-MS analysis was supplied by Sigma-Aldrich (UK).
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6

Quantification of Organic Analytes in Plasma

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3–Heptanone was provided from Sigma–Aldrich (St. Louis, USA). Sodium valproate powder was a gift from Rouz Darou Pharmaceutical Co. (Tehran, Iran). Methanol was also supplied from Sigma–Aldrich. Carbon tetrachloride, trifluoroacetic acid, 1,1,2,2–tetrachloroethane (1,1,2,2–TCE), 1,2–dichloroethane (1,2–DCE), and chloroform were provided from Merck (Darmstadt, Germany). Deionized water was provided from Ghazi Pharmaceutical Company (Tabriz, Iran). Appropriate amounts of the target analytes were dissolved in Methanol and stock solutions (C=1000 mg L–1, each analyte) were obtained. For the preparation of working standard solution, the appropriate volume of stock solution was spiked into drug-free plasma.
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7

Volatile Compound Analysis of Biscuits

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Biscuits were ground in a mortar and weighed (3 g ± 0.001 g) in a 20 mL vial, then 6 mL of water and 20 µL of internal standard (3-heptanone, Sigma, Saint Louis, USA, at 0.01 mg/L in methanol, Laboratory reagent grade, Fisher Scientific, UK) were added. All the vials were sealed by silicon lid with PTFE septa and aluminium crimp caps.
Some fermentation issues were observed after 4 h so the sample order was randomised to avoid systematic changes during the day and each vial was analysed 1 h after preparation. 5 replicate measurements were carried out on each type of biscuit.
Before volatile extraction, the sample was pre-heated for 15 min using the GC agitator.
The extraction of volatile compounds was carried out by exposing a 1 cm length of StableFlex SPME fibre with a 50/30 μm divinylbenzene/Carboxen/polydimethylsiloxane coating (DVB/CAR/PDMS) in the headspace of the sample at 35 °C for 10 min. The fibre was then desorbed for 15 min in the injection port of the gas-chromatograph (Trace GC Ultra -Thermo Scientific) operating in split-less mode.
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8

Volatile Profiling of Nut-Based Milk Beverages

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All samples of nut-based milks (i.e., almond beverages, walnut beverage, peanut beverage, almond and cacao beverage) were obtained from the local market in Thessaloniki, Greece. All samples were stored in the refrigerator (+4 °C). Butyrophenone (purity ≥99%) was used as internal standard (IS) solution (Sigma-Aldrich, St. Louis, MO, USA). A stock solution of IS was prepared in methanol (Panreac, Barcelona, Spain) at a concentration of 1000 mg L−1. A stock standard solution containing heptane (purity >99%, Sigma-Aldrich), a-pinene (purity >95%, Fluka, St. Gallen, Swiss), toluene (purity >99.8%, Sigma-Aldrich), 2-methylpyrazine (purity >99%, Sigma-Aldrich), 3-heptanone (purity >98%, Sigma-Aldrich), heptanal (purity >95%, Sigma-Aldrich), 2-octanone (purity >98%, Sigma-Aldrich), 1-heptanol (purity >98%, Sigma-Aldrich), benzaldehyde (purity >99%, Sigma-Aldrich) and 1-octanol (purity >99%, Sigma-Aldrich) was prepared in methanol (concentration of each analyte 1000 mg L−1) and used for the identification of the volatile compounds and method validation. Τhe stock solution was stored in the refrigerator (+4 °C) and it was found stable for up to 2 months. Working standard solutions were prepared daily by diluting appropriate amount of stock standard solution and IS solution in distilled water.
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9

Foxtail Millet Cooking Optimization

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Four varieties of foxtail millet (Jingu 21, Jingu36, Daqinggu, Zhishenggu) were harvested in 2014, and dehusked using a rice huller (JLGJ-45, Hangzhou HR, China).
Jingu 21 millet grains were milled using a grinder (DēLonghi, KG49, Germany). All samples were stored at 4 ℃.
Millet (1.5 g), ultra-pure water (Pur1te 'Select' DI Water System, UK) (7.5 ml) and 20 µl of internal standard (5 mg) 3-heptanone (Sigma, Saint Louis, USA) in 100 ml
methanol (Laboratory reagent grade, Fisher Scientific, UK) were added to a sample vial (20 ml, 75.5 x 22.5 mm, Fisherbrand). Prepared samples were heated in the GC incubator at 100 ℃. Standard cooking time was 20 min, but additional tests were done at 0, 10, 20, 30, 40 min. The pH of the water was adjusted to pH6, pH7, pH8 by 0.1M HCl and 0.1M NaOH; Two sizes of processed millet (millet grain, millet flour) were compared.
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