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20 protocols using deuterated chloroform cdcl3

1

Synthesis of Polymer Nanocomposites

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Bisphenol AF (>98%), 4,4′-oxydianiline (>98%), and 1-(2-furyl)methylamine (99%) were purchased from TCI America (Portland, OR, USA). Paraformaldehyde (>95%), tetrahydrofuran (≥99.9%), and TLC Silica gel 60 F254 (100 glass plates, 2.5 cm × 7.5 cm) were obtained from Sigma Aldrich (Burlington, MA, USA). Chloroform and sodium hydroxide (NaOH) were received from Fisher Scientific Company (Waltham, MA, USA). Deuterated Chloroform (CDCl3) (99.8%) was purchased from Cambridge Isotope Laboratories., Inc. (Tewksbury, MA, USA). Glycidyl isobutyl POSS (EP0418) was purchased from Hybrid Plastics Inc. (Hattiesburg, MS, USA). Woven 3M Nextel 312 ceramic fabric (Style AF-40, 5 harness satin weave, 1800 denier, heat cleaned) was purchased from Bristal Metal Products, Inc. (Westlake, OH, USA). All chemicals were used as received.
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2

Formulation and Characterization of TPGS-based Paclitaxel Nanoparticles

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D-α-Tocopherol polyethylene glycol 1000 succinate (TPGS1000), ε-Caprolactone (97%), and stannous octoate were purchased from Sigma-Aldrich (St. Louis, MO, USA). D-α-Tocopherol polyethylene glycol 2000 succinate (TPGS2000), D-α-Tocopherol polyethylene glycol 3500 succinate (TPGS3500), and D-α-Tocopherol polyethylene glycol 5000 succinate (TPGS5000) were obtained from Wuhan Jason Biotech Co., Ltd. (Wuhan, Hubei, China). Paclitaxel (99%) was purchased from Shaanxi Sciphar Biotechnology Co., Ltd. (Xianyang, Shijiyiuan, China). Ebetaxel® (300 mg/50 mL, concentrate for infusion; Ebewe Pharma, Unterach, Austria; Lot# HN5538), a generic of Taxol® approved by the US FDA, was obtained from King Khalid University Hospital Pharmacy (Riyadh, Saudi Arabia). Deuterated chloroform (CDCl3, 99.8%) was purchased from Cambridge Isotope Laboratories Inc. (Tewksbury, MA, USA). Polysorbate 80 (Tween 80) was purchased from Bio Basic Inc. (Markham, ON, Canada). Potassium dihydrogen orthophosphate, dipotassium hydrogen orthophosphate, and potassium chloride were obtained from BDH Chemical Ltd. (Poole, England). Acetonitrile, methanol, and water were all HPLC grade and were purchased from BDH Chemical Ltd. (Poole, England). All other chemicals were reagent grade.
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3

Alginate Extraction from Saccharina latissima

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Sodium alginate was extracted from the brown algae Saccharina latissima using a cyclic fractionation process in which diluted sodium citrate was used in 18 sequential extractions from the same biomass [4 (link)]. The alginate fraction used in this work was recovered, by acid precipitation followed by centrifugation, from the 16th extraction cycle. The algae were cultivated on the Swedish west coast and harvested on 17 May 2016, from a cultivation site at the Sven Lovén Centre for Marine Science (University of Gothenburg). The precise extraction protocol is described in a previous work [8 (link)]. Commercial sodium alginate, sodium hydroxide (≥97% ACS reagent, CAS: 9005-38-3), maleic anhydride (MA) (≥99.0% puriss), n-dodecanol (DD) (≥98%, reagent grade), calcium chloride dihydrate (CaCl2) (≥99% ACS reagent), sodium oxalate (≥99.5% ACS reagent), and phytic acid (≥90% phosphorus basis) were purchased from Sigma-Aldrich, Sweden. Deuterated chloroform (CDCl3) (99.96%) was purchased from Cambridge Isotope Laboratories, U.S.A. Linseed oil was purchased from Slöjdetaljer, Sweden, and produced by Eskil Åkerberg AB, Staffanstorp, Sweden.
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4

Synthesis of Organic Compounds

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All reagents were purchased from TCI chemicals, Aldrich and Fisher. Deuterated chloroform (CDCl3) was purchased from Cambridge Isotope Laboratories. Silica gel for column chromatography was purchased from Silicycle. All chemicals were used as received.
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5

Synthesis of Polymeric Brushes via ATRP

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n-Butyl acrylate (BA, 99%, Aldrich, St. Louis, MO, USA) was passed through basic alumina column to remove radical inhibitors prior to use. Anisole (Aldrich, 99%), nitrosobenzene (NBz, 99%, Aldrich, St. Louis, MO, USA), α-bromoisobutyryl bromide (BiBBr, 98%, Aldrich, St. Louis, MO, USA), pentaerythritol (for synthesis Aldrich, St. Louis, MO, USA), tin (II) ethylhexanoate (Sn(EH)2, 98%, Aldrich, St. Louis, MO, USA), tetrahydrofuran (THF, ACS grade, Fisher Scientific, Hampton, NH, USA), copper(II) bromide (CuBr2, 99%, Aldrich, St. Louis, MO, USA), N,N-dimethylformamide (DMF, ACS grade, Fisher Scientific, Hampton, NH, USA), deuterated chloroform (CDCl3, 99.8%, Cambridge Isotope Laboratories, Tewksbury, MA, USA), and tris [2-(dimethylamino)ethyl]amine (Me6TREN, Aldrich, St. Louis, MO, USA) were used as received.
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6

Characterization of Lipid Mixtures for Biomembrane Studies

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N-Acyl-4-sphingenyl-1-O-phosphorylcholine (egg sphingomyelin, egg SM), 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphoethanolamine (16:0/18:1 PE, POPE) 1-palmitoyl-2-oleoyl-sn-glycero-3-phospho-(1'-rac-glycerol) (sodium salt) [16:0/18:1 PG, POPG] were purchased from Avanti Polar Lipids (Alabaster, AL) and used as received (Fig. S5). Lipid stock solutions were prepared by dissolving the dry lipid powder in either HPLC-grade chloroform (ACP Chemicals Inc., Saint Lonard, QC) or in a combination of HPLC-grade chloroform and HPLC-grade methanol (Sigma-Aldrich, Oakville, ON) in a 2:1 ratio respectively. Methyl-beta-cyclodextrin (mβ CD) was purchased from Sigma-Aldrich (Oakville, ON) and prepared as a 35 mmol/L (mM) stock solution in ultrapure H 2 O. The sucrose was purchased from Sigma-Aldrich (Oakville, ON) and prepared as a 0.632 M stock solution in ultrapure H 2 O. Sodium chloride was purchased from Sigma-Aldrich (Oakville, ON) and prepared as a 20 mM solution in D 2 O. Praseodymium (III) nitrate hexahydrate (Pr(NO 3 ) 3 • 6H 2 O) [Pr 3+ ] was purchased from Sigma-Aldrich (Oakville, ON) and prepared as 40 mM stock solution in D 2 O. The deuterated chloroform (CDCl 3 ) was purchased from Cambridge Isotopes (Andover, MA). Ultrapure H 2 O was obtained from a Milli-Q purification system (Millipore-Sigma, Oakville, ON) and 99.9% D 2 O was purchased from Cambridge Isotopes (Andover, MA).
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7

Enzymatic Modification of Cod Liver Oil

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Arctic cod liver oil was purchased from Nordic Naturals (Watsonville, CA, USA). Lipozyme RM IM (Rhizomucor miehei lipase, immobilized on anion exchange resin), Lipozyme TL IM (lipase from Thermomyces lanuginosa) and Novozyme 435 (Lipase acrylic resin from Candida antarctica B) were generous gifts from Novo Nordisk A/S (Bagsvaerd, Denmark). Sodium methoxide, sodium hydroxide, and boron trifluoride-methanol solution (14% in methanol) were obtained from Sigma-Aldrich (Singapore).
Acetone, hexane, ethanol and methanol were acquired from RCI Labscan Limited (Bangkok, Thailand). Deuterated chloroform (CDCl 3 ) containing tetramethylsilane (TMS, v/v 0.03%) was purchased from Cambridge Isotope Laboratories Inc. (Tewksbury, MA, USA).
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8

Extraction of Lipids from Salmon Roe

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All chemicals and reagents used in the present work were of analytical grade of the highest purity available. Methanol and chloroform were from Merck (Darmstadt, Germany), and deuterated chloroform (CDCl3, 99.8%) was obtained from Cambridge Isotope Laboratories, Inc., Tewksbury, MA, USA. Fresh, salted-dried, and salted-fermented salmon roe samples were collected for analysis on 0, 20, and 30 d, respectively, of processing. Fermentation and salting of salmon roe were carried out based on the methods described previously [5 (link),6 (link)]. Roe samples then were freeze dried and ground prior to extraction of the lipids.
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9

Quantitative Analysis of Salmon Roe Lipids

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The 13C NMR analysis method used was based on a previously reported study [7 (link),10 (link),11 (link),14 (link)], which reported a carbonyl peak at δ 175.0 and characteristic five aliphatic carbon signals at δ 34.2, 31.2, 24.6, 22.3, and 13.9. Lipid (180 mg) extracted from the salmon roe samples was dissolved in 700 μL of deuterated chloroform (CDCl3; Cambridge Isotope Laboratories, Inc., USA) and then transferred to a 5 mm NMR tube. The 13C NMRs (100 MHz) were conducted using a Varian 400 MHz VNMRS instrument (Varian, Inc., Pullman, WA, USA) using a 5 mm OneprobeTM, and the running conditions used were those as described previously [7 (link),14 (link),42 ]. Chemical shifts for both carbon and proton were referenced to a region peak of CDCl3 at 77.06 ppm. The NMR spectra were analyzed using MestReNova version 12.0 software (Mestrelab Research, Bajo, Santiago de Compostela, Spain). Peak assignment identification was carried out according to previously reported literature [43 (link)]. Area percentage of fatty acids was obtained from the area integrator response of the NMR spectra (MestReNova version 12.0 software, Mestrelab Research, Bajo, Santiago de Compostela, Spain).
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10

Fatty Acid Composition Analysis of Shrimp Lipids

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L. vannamei shrimp (Huazhong Agricultural University Agricultural Products Market, Wuhan, China), and high-oleic sunflower oil (Zhongliang Co., Ltd., Beijing, China).
Anhydrous ethyl ether, isopropyl alcohol, potassium hydroxide, chloroform, methanol, potassium thiocyanate, ferrous chloride, p-anisidine, hydrochloric acid, and glacial acetic acid were purchased from Sinopharm Chemical Reagent Co., Ltd. (Shanghai, China). Isooctane, 2,4-dinitrophenylhydrazine, and phenolphthalein were from Shanghai Macklin Biochemical Co., Ltd. (Shanghai, China). Deuterated chloroform (CDCl3) was acquired from Cambridge Isotope Laboratories Inc. (Andover, MA, USA).
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