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8 protocols using nh4oh solution

1

Synthesis and Characterization of PEG-Coated MNPs

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Melanin, amine-PEG5000-amine, sodium hydroxide, hydrochloric acid, and NH4OH solution were purchased from Sigma-Aldrich. Dulbecco’s modified Eagle medium (DMEM), 10% fetal bovine serum (FBS) and phosphate buffered saline (PBS) were purchased from Gibco. The A431 cell line was obtained from the American Tissue Culture Collection. 64CuCl2 was purchased from the Department of Medical Physics, University of Wisconsin at Madison. The synthesis of polyethylene glycol modified MNPs (PEG-MNPs) was performed according to previous work.24 (link)
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2

Gold Nanoparticle Synthesis Protocol

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Tetraethyl orthosilicate (TEOS, 99.999%), Igepal CO-520, NH4OH solution (ACS reagent, 28–30%), gold chloride trihydrate (HAuCl4·3H2O, ≥99.99% trace metal basis), hydroxylamine hydrochloride (NH2OH·HCl, 99.995%, trace metal basis), poly-l-histidine hydrochloride (PLH, molecular weight ≥ 5000), and mPEG thiol (molecular weight ∼ 6 kDa) were purchased from Sigma-Aldrich. Cyclohexane (spectroscopy grade) was purchased from Acros Organics. Sodium hydroxide (certified ACS) was purchased from Fisher Scientific. Nanopure water (18 MΩ) was used for all aqueous-phase syntheses.
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3

Synthesis of Superparamagnetic Nanoparticles

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Iron(II) chloride tetrahydrate (FeCl2·4H2O) (purity: 98%), iron(III) chloride hexahydrate
(FeCl3·6H2O) (purity: 97%), NH4OH solution (28–30% NH3 in H2O), and
oleic acid (purity: ≥93%) were purchased from Sigma-Aldrich
and used in the synthesis of SPN and OA-SPN. Besides, acrylamide (purity:
98%), potassium persulfate (K2S2O8) (purity: 98%), ethanol, and acetone were also obtained from Sigma-Aldrich
and used for the synthesis of SPN@PAM. In addition, polyacrylamide
(PAM) with an average molecular weight of 20 000–30 000
g/mol was used in the fabrication of SPN-PAM. Finally, n-decane was purchased from Sigma-Aldrich and used as the oil model
in EOR injection.
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4

Synthesis of Silica Nanoparticles

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The synthesis of silica nanoparticles (NPs-SiO2) was carried out following the method previously described by Zhou et al. in 2014 (ref. 16 (link)) (Scheme 1). A solution (A) consisting of 316 g ethanol, 56 g H2O Milli-Q® and ammonium hydroxide solution (NH4OH) was prepared. Meanwhile, 18.6 g of Tetraethylorthosilicate (TEOS) and 18.6 g of ethanol were mixed (solution B). Solution A was stirred for 10 min with reflux at 40 °C, while solution B was stirred for 5 min at room temperature. Solution B was then added to solution A and left under stirring with reflux at 40 °C for 30 min. The resulting solution was centrifuged in an AVANTI J-25 XP centrifuge at 12 000 rpm for 10 min and washed successively with water at the same speed and time, until neutral pH. Finally, the solid obtained was dried at 60 °C overnight. The amount of ammonium hydroxide used was varied between 3.5 and 29 g, depending on the desired particle size. Tetraethylorthosilicate (98%) and NH4OH solution (28–30% NH3 in H2O) were purchased from Sigma-Aldrich. Absolute ethanol was supplied by Scharlab. Pure silica nanoparticles were labelled as NPs-SiO2.
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5

Derivatization of Compounds using FMOC

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FMOC reagent (20 mg/mL ACN) was prepared by diluting 5 g of FMOC chloride (HPLC derivatization, ≥ 99.0 %, Sigma Aldrich, St. Louis, MO, USA) in 250 mL of ACN. Borate buffer reagent (50 mmol) was prepared by diluting 4.8 g of sodium tetraborate decahydrate (ACS reagent, ≥ 99.5 %, Sigma Aldrich St. Louis, MO, USA) in 250 mL of H2O. Ammonium hydroxide (NH4OH) 2 % solution was prepared by diluting 5 mL of NH4OH solution (28 % to 30.0 % NH3 basis, Sigma Aldrich St. Louis, MO, USA) in 68 mL of H2O.
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6

Melanin Functionalization and Cell Viability

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The
following reagents were acquired and
used as received: melanin (Sigma-Aldrich), sodium hydroxide (Sigma-Aldrich),
hydrochloric acid (37 wt %, Sigma-Aldrich), NH4OH solution
(28 wt %, Sigma-Aldrich), amine-PEG5000-amine (NH2-PEG5000-NH2, 5 kDa, Laysan Bio), dimethylthiazolyl-diphenyltetrazolium
(MTT; Biotium), phosphate buffered saline (PBS, Gibco), and agarose
(Invitrogen). Millipore water (at 18 MOhm) was used.
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7

Dextran-Coated Iron Oxide Nanoparticles

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The starting materials, FeCl3•6H2O,
FeCl2•4H2O, and NH4OH solution were purchased from Merck. Magnetite
nanoparticles were synthesized according to the literature with some modifications (19 (link))
through the alkaline coprecipitation method using iron (II) and (III) chlorides. Briefly,
1.6 g FeCl3•6H2O and 0.6 g FeCl2•4H2O were
grinded and then added to a beaker containing 50 ml deionized water. The beaker was kept
in an ultrasonic bath for 30 minutes. The prepared solution was transferred into a
three-neck flask and agitated vigorously under nitrogen gas atmosphere. After 5 minutes’
agitation, 30 ml NH4OH was added dropwise during 45 minutes. Finally, the suspension was
kept at 75-80°C for 80 minutes. The nanoparticles were separated magnetically and washed
several times to adjust the pH. The collected iron oxide nanoparticles were dispersed in a
5% dextran solution and stirred for 5 hours at 75°C. The solution containing
dextran-coated iron nanoparticles, was centrifuged at 11000 rpm for 15 minutes to
eliminate the larger particles.
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8

Quantitative Analysis of F and HMF in Milk/Baby Food

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F and HMF (analytical-grade), acetonitrile and methanol (HPLC-grade), ethyl acetate, ethanol (EtOH), isopropanol, acetone, FeCl3·6H2O, FeCl2·6H2O, terephthalic acid (H2BDC), K3[Fe(CN)6], aniline, ammonium persulfate, pyrrole, NaOH, NaCl, (Zn(OAc)2), N,N-dimethylformamide (DMF), acetic acid, and NH4OH solution (25% w/v) were purchased from Merck (Darmstadt, Germany) or Sigma-Aldrich (Germany). A Milli-Q system (Millipore, MA, USA) was employed to prepare deionized water (DI). The real samples (dried milk/baby food) were obtained from the local drug stores (Tehran, Iran) and maintained in a refrigerator (4 °C) before analysis.
Stock solutions of F and HMF (1000 mg L−1) were prepared in HPLC-grade methanol. The mixed working solutions were prepared by dilution of the proper volumes of the stock solution in DI water. To prepare the Carrez solution, 10.6 g K3[Fe(CN)6] was dissolved in 100 mL DI water. Carrez solution II was obtained by mixing 21.9 g Zn(OAc)2 and 3 mL HOAc in a 100 mL volumetric flask and adjusting the volume by DI water.
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