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7 protocols using 4 methyl 2 pentanone

1

Preparation of Volatile Organic Compound Standards

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Individual samples were prepared by injecting desired liquid volumes of 2-butanone, 2-hexanone, ethyl acetate and 4-methyl-2-pentanone (Sigma Aldrich, St Louis, MO) into each sample bag (SKC Tedlar® Sample bag, SKC Inc., Eighty Four, PA) filled with 3 L of ultra high purity nitrogen (Airgas, Radnor, PA). These bags were maintained for more than 10 min at room temperature to equilibrate analytes into the gas phase to achieve the stock concentrations (1000 ppm). Serial dilution was performed from the stock concentration to achieve 100 ppm concentration of each chemical. Each gas phase chemical was sampled into a gas tight 1 mL glass syringe (Hamilton Co., Reno, NV) from the final concentration (100 ppm) and introduced separately into the inlet of the differential mobility spectrometer using a syringe pump with a dilution nitrogen gas flow. The final concentration of each chemical at the DMS cell inlet was 500 ppb. The bags with chemical mixtures were prepared by adding each new chemical to the bag followed by serial dilution. Therefore, the final concentration of each chemical in a mixture was ~ 500 ppb.
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2

Volatile Compound Analysis via SPME

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Gas mix 1 : 3 18O2 oxygen (98%) and 14N2 nitrogen was from CK Gas Products Ltd. (Hook, UK). hexanoic acid-2, 2-D2 acid (98 atom % D); hexanoic-D11 acid (98 atom % D); hexanoyl-CoA trilithium salt hydrate (C6:0); hexanoylcarnitine, hexanoic acid, octanoic acid, 4-methyl-2-pentanone (MIBK) >99%, cyclohexanone 99.8%, 2-pentanone 99.5%, 2-pentanol 98%, ethyl 3-oxohexanoate (ethyl butyrate) 98% purities, and pentane were from Sigma-Aldrich (Gillingham, UK). Hexane (HPLC grade) was from Fisher Scientific UK Ltd. (Loughborough, UK). Blue cheese and margarine were obtained commercially. In preliminary studies (Section 3.2), 250 μL of a 1 in 2,000 dilution of cyclohexanone in water was added as internal standard (IS). In later experiments (Sections 3.3 and 3.4), the IS was 20 μL of a 1 in 1,000 dilution of MIBK in water. Working solutions of hexanoic acid (1H or deuterated) were prepared as dilutions in melted margarine (1 μL/mL; 8 mmol/L).
Carboxen-polydimethylsiloxane 75 μm film thickness solid-phase microextraction (SPME) fibres and SPME fibre syringe holders were from Supelco (Poole, UK); headspace (HS) vials (22 mL) with soft silicone rubber seals (20 mm diameter) and aluminium caps were from Alltech Associates Ltd. (Carnforth, UK). Water was deionised by reverse osmosis.
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3

Comprehensive Lipid Profiling Analysis

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Sodium methylate (0.5 mol L−1 methanolic solution, HPLC grade), sulphuric acid (98%), acetic acid glacial (99.5%), sodium thiosulphate (0.1 mol L−1), starch solution, and n-hexane (99%, GC grade) were obtained from Panreac (Barcelona, Spain). Standards for GC analysis (99%) of methyl tridecanoate, oleic, linoleic, stearic, and palmitic acid methyl esters, petroleum ether (≥95%), methanol (≥99.8%), potassium iodide, chloroform (≥99.8%, for HPLC), acetic acid, hydrochloric acid, isooctane, potassium iodate, p-anisidine reagent, internal standard 4-methyl-2-pentanone, and hexanal (98%) were acquired from Sigma-Aldrich Inc. (St. Louis, MO, USA). All chemicals used were of analytical grade.
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4

Thiol-Epoxy Photocurable Hybrid Polymers

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Acrylated epoxidized soybean oil (AESO, an average number of acryloyl groups per molecule 2.7 and 0.3 of epoxide groups), benzene-1,3-dithiol (1,3BDT), pentaerythritol tetra(3-mercaptopropionate) (PETMP), 1-methylimidazole (1MI), and 4-methyl-2-pentanone were purchased from Sigma-Aldrich (Darmstadt, Germany). Epoxidized linseed oil (ELO, having an average number of 6 epoxy groups per molecule) was purchased from Chemical Point (Oberhaching, Germany). Photoinitiator ethyl(2,4,6-thimethylbenzoyl) phenyl phosphinate (TPOL) was purchased from Fluorochem (Hadfield, Derbyshire, UK). All materials were used as received.
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5

Antioxidant Extraction from Guara Almond Skins

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Water (ultrapure grade) and ethanol (HPLC grade) were acquired from Merck (Madrid, Spain). Hexanal (98%), p-anisidine reagent (99%), 2,2-diphenyl-1-picrylhydrazyl (DPPH), sodium chloride, methanol (HPLC grade) and n-hexane (96%, GC grade) were supplied by Sigma-Aldrich (Madrid, Spain). Petroleum ether, sodium methylate, sulphuric acid (98%), acetic acid, potassium iodide, sodium thiosulfate (0.1 M), chloroform, isooctane were of analytical or chromatographic grade and were purchased from Panreac (Barcelona, Spain). Standard compounds such as linoleic (C18:2), oleic (C18:1), palmitic (C16:0), palmitoleic (C16:1), stearic (C18:0) and tridecanoic (C13) acid methyl esters; and 4-methyl-2-pentanone were acquired from Sigma-Aldrich (Madrid, Spain) in the purest available form. A commercial poly(ε-caprolactone) PCL-CAPA 6800 (Mn = 80,000, density = 1.1 g cm−3) was supplied in pellets by Perstorp Holding AB (Sweden). Guara almond skins (AS) were kindly supplied by Almendras Llopis (Alicante, Spain).
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6

Headspace Extraction of Volatile Compounds in Raw Lamb Meat

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A divinyl benzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber 50/30 μm (Supelco, Bellefonte, PA, USA) was used to extract headspace volatile compounds from raw lamb meat. Prior to use, the fiber was conditioned following the manufacturer’s recommendations. Approximately, 2 g of lamb meat from different parts of the lamb legs were placed in a 20 mL crimp-cap vial (72 × 20 mm) equipped with PTFE/silicone septa. Then, 10 μL of an internal standard (4-methyl-2-pentanone, of initial concentration C = 640 ng/mL, Sigma Aldrich (Darmstadt, Germany)) was added at the walls of the vial, and the vial was wrapped. It was vortexed for 5 min in order for the internal standard to be spread homogenously at the surface of raw lamb meat. The vial was then maintained at 50 °C in a water bath under stirring at 600 rpm during the entire extraction procedure, which was 30 min (15 min was the equilibration time and 15 min was the adsorption time). It should be stressed that when the heating of the raw meat product is somehow “mild” during analysis, the volatile profile can be considered as pure information, originating from raw meat. Volatile compounds analysis was carried out on day 1, day 5, and day 9 of storage. Each sample was run in duplicate (n = 2).
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7

Chloroform-Based Compound Extraction

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chloroform-d (99.8%), 4-methyl-2-pentanone (internal standard), chloroform, hexane, diethyl ether, methanol and 2-propanol (HPLC grade) were purchased from Sigma Aldrich (Milan, Italy). SPE cartridges (GracePure TM SPE C18-Max) were purchased from SepaChrom (Rho MI, Italy).
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