The mobile phase consisted of HPLC-grade acetonitrile from VWR (Radnor, PA, USA) and all water used in this study was deionized water with a conductivity of 18.2 MΩ cm−1 from a Milli-Q Advantage A10 water purification system (Merck Millipore, Darmstadt, Germany). Trimethylamine solution (44 wt% in H2O, CAS# 75-50-3), triethylamine (≥ 99.5%, CAS# 121-44-8), tripropylamine (≥ 98%, CAS# 102-69-2), tributylamine (≥ 99.5%, CAS# 102-82-9), and acetic acid (99.8–100.5%, CAS# 64-19-7) were all purchased from Sigma-Aldrich (St. Louis, MO, USA). All oligonucleotide samples were purchased from Integrated DNA Technologies (Leuven, Belgium) as “1 μmole DNA Oligo” products delivered in lyophilized and desalted form and used without further purification. Their absolute purity was not established, as it varies with length and composition, but can be expected to be high in the case of a pentamer given a synthesis coupling frequency of > 99%. The general structure of the pentamer used in this study is shown in Electronic Supplementary Material (ESM) Fig. S1 .
Tripropylamine
Manufactured by Merck Group
Sourced in United States
Tripropylamine is a colorless, flammable liquid chemical compound. It is used as a reagent and catalyst in various industrial and laboratory applications.
Automatically generated - may contain errors
Lab products found in correlation
Triethylamine, by Merck Group (2 mentions)
Tributylamine, by Merck Group (1 mentions)
Hplc grade acetonitrile, by Avantor (1 mentions)
Milli q advantage a10, by Merck Group (1 mentions)
Trimethylamine solution, by Merck Group (1 mentions)
Acetic acid, by Merck Group (1 mentions)
Human hemoglobin, by Merck Group (1 mentions)
Angiotensin 2, by Merck Group (1 mentions)
Propylamine, by Merck Group (1 mentions)
Trimethylamine, by Merck Group (1 mentions)
Ms grade trypsin, by Thermo Fisher Scientific (1 mentions)
Schiff s reagent, by Merck Group (1 mentions)
Xylene, by Thermo Fisher Scientific (1 mentions)
Acetone, by Thermo Fisher Scientific (1 mentions)
Jeffamine m 2070, by Huntsman (1 mentions)
Sulfuric acid, by Thermo Fisher Scientific (1 mentions)
Boron trifluoride diethyl etherate, by Thermo Fisher Scientific (1 mentions)
Hydrobromic acid, by Merck Group (1 mentions)
Grubbs catalyst 1st generation, by Merck Group (1 mentions)
P toluenesulfonyl hydrazide, by Merck Group (1 mentions)
6 protocols using tripropylamine
1
Optimized HPLC Analysis of Oligonucleotides
2
Quantitative Hemoglobin-Aldehyde Analysis
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Human hemoglobin, Angiotensin II, trimethylamine, tripropylamine, propylamine and Schiff’s reagent were purchased from Sigma-Aldrich. MS-grade trypsin was obtained from Thermo scientific (Rockford, IL, USA). Triethylamine and 3 Å Molecular sieves (8–12 mesh beads) were procured from EMD Millipore (Darmstadt, Germany). Acetaldehyde and propionaldehyde were purchased from TCI America (Portland, OR, USA).
3
Synthesis and Purification of PPMA-g-Jeffamine
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Example 1
Synthesis.
10 grams PP-g-MA (Aldrich) (average Mw approximately 9,100 by GPC, average Mn approximately 3,900 by GPC, maleic anhydride 8-10 wt %) and 10 grams Jeffamine M2070 (Huntsman), were suspended in 200 ml Xylene (Fisher), and 2 g Tripropylamine (Sigma-Aldrich), was added afterward. The suspension was heated up to 125° C. for 48 hours. No initiator was used because it is a N-imidation reaction.
Purification.
Graft copolymer solution in Xylene was precipitated in acetone (Fisher), rinsed with acetone (Fisher) and solvent extraction with acetone (Fisher) for 24 hours. Tripropylamine is removed during this step. Purified material was dried in the vacuum oven overnight.
Yield.
PPMA-g-Jeffamine (e.g., PPMA-g-PEO-PPO) was ˜85% after purification based on the starting amount of PP-g-MA.
4
Synthesis of Functionalized Adamantane Derivatives
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2,2′-(Adamantane-1,3-diyl)diacetic
acid (Sigma, 97%), boron trifluoride diethyl etherate (Acros, 48%
in Et2O), 4-chloro-1-butene (Acros, 98%), 9-chloro-1-nonene
(flourochem, >95%), 8-chloro-1-octene (flourochem, >95%), CDCl3 (Sigma, 99.8%), copper(II) chloride (CuCl2, Acros,
anhydrous 99%), Grubbs Catalyst 1st Generation (Sigma, 97%), HDPE
(Alfa Aesar, Mw = 125 kDa), hydrobromic
acid (Sigma, 47% in H2O), lithium aluminium hydride (Acros,
2.4 M in THF), magnesium purum, for Grignard reactions (Sigma, >99.5%),
1-phenyl-1-propyne (Acros, 99%), sulfuric acid (Fischer scientific,
>95%), THF anhydrous (Sigma, >99.9% inhibitor free), p-toluenesulfonyl hydrazide (Sigma, 97%), tripropylamine
(TCI, >98%), o-xylol anhydrous (Sigma, 97%) were
used and flash column
chromatography was performed on silica gel 60 (Macherey-Nagel GmbH,
40–63 μm, 230–400 mesh).
acid (Sigma, 97%), boron trifluoride diethyl etherate (Acros, 48%
in Et2O), 4-chloro-1-butene (Acros, 98%), 9-chloro-1-nonene
(flourochem, >95%), 8-chloro-1-octene (flourochem, >95%), CDCl3 (Sigma, 99.8%), copper(II) chloride (CuCl2, Acros,
anhydrous 99%), Grubbs Catalyst 1st Generation (Sigma, 97%), HDPE
(Alfa Aesar, Mw = 125 kDa), hydrobromic
acid (Sigma, 47% in H2O), lithium aluminium hydride (Acros,
2.4 M in THF), magnesium purum, for Grignard reactions (Sigma, >99.5%),
1-phenyl-1-propyne (Acros, 99%), sulfuric acid (Fischer scientific,
>95%), THF anhydrous (Sigma, >99.9% inhibitor free), p-toluenesulfonyl hydrazide (Sigma, 97%), tripropylamine
(TCI, >98%), o-xylol anhydrous (Sigma, 97%) were
used and flash column
chromatography was performed on silica gel 60 (Macherey-Nagel GmbH,
40–63 μm, 230–400 mesh).
5
Sensitive Electrochemical Biosensor Development
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Titanium(IV) isopropoxide (Ti(OR)4, R = CH(CH3)2, 99.999%), Nafion (perfluorinated ion exchange resin, 5 wt.% in lower aliphatic alcohols and water contains 15~20% water), tripropylamine (TPA, 99%), tris(2,2′-bibpyridyl)dichlororuthenium(II) hexahydrate (Ru(bpy)3Cl2·6H2O, 98%), and beta-nicotinamide adenine dinucleotide reduced disodium salt hydrate (β-NADH) and human serum were purchased from Sigma-Aldrich. 2-Propanol (≥99.9%) (Fluka, Germany) and hydrochloric acid (35–37%) (Samchun, Korea) were used to prepare sol-gel derived titania. Graphene nanoplatelets were obtained from Cheap Tubes Inc. (Grafton, VT, USA). Carbon nanotube, multi-walled (>99% MWCNT, diameter: 6~13 nm, and length: 2.5~20 µm) was obtained from Sigma-Aldrich. All chemicals were used as received without any further purification. All experimental solutions were prepared using 0.05 M phosphate buffer solution at pH 7. Water for all solutions was purified using a Milli-Q water purification system (Bedford, MA, USA).
6
Exosomal Protein Detection Protocol
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Rabbit monoclonal antibody CD63 and exosomal protein CD63, CD81, CD69, bovine serum albumin (BSA), carcino-embryogenic antigen (CEA), alpha fetoprotein (AFP), haptoglobin (Hp), sodium azide, potassium chloride, potassium ferrocyanide, potassium ferricyanide, tris (2,2ʹ-bipyridyl) dichlororuthenium(II) hexahydrate, tripropylamine, trisdisodium phosphate, and monosodium phosphate, nanocomposite binding agent, carbon nano chips (CNCs), 5% NAF solution were purchased from Sigma-Aldrich (USA). Iron oxide (Fe3O4) nanoparticles were procured from US Research Nanomaterials, Inc. (Houston, USA).
All solutions were prepared using freshly obtained Milli-Q water (deionised with specific resistance ∼18 M.cm -1 ). All the experiments were performed at the room temperature (RT) (21 ± 0.5 °C).
All solutions were prepared using freshly obtained Milli-Q water (deionised with specific resistance ∼18 M.cm -1 ). All the experiments were performed at the room temperature (RT) (21 ± 0.5 °C).
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