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12 protocols using montmorillonite

1

Pluronic F-127 Hydrogel Synthesis

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Pluronic F-127 (Sigma-Aldrich), anhydrous toluene (Wako, 99.5%), trimethylamine (Wako, 99.0%), methacryloyl chloride (TCI, 90%), diethyl ether (Wako, 99.5%), montmorillonite (The Clay Science Society of Japan), pentaethylene glycol monodecyl ether (C10E5) (Sigma Aldrich, 97.0%), potassium carbonate (K2CO3) (Wako, 98.5%), niobium(v) oxide (Nb2O5) (Wako, 99.9%), hydrochloric acid (HCl) (Wako, 35.0%), tetrabutylammonium hydroxide solution (TBAOH) (Sigma-Aldrich, 40 wt%), and 2-hydroxymethyl propiophenone (TCI, 96.0%) were used in this study.
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2

Synthesis of Hydroxyapatite Nanocomposites

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All the chemicals used were analytical grade and used without further purification. Ammonium hydroxide (NH4OH solution, 25%, Sigma Aldrich), calcium nitrate tetrahydrate (Ca(NO3)2·4H2O, 98% Sigma Aldrich), di-ammonium hydrogen orthophosphate ((NH4)2HPO4, 98% Sigma Aldrich) were used to synthesis neat HAP. Montmorillonite (Sigma Aldrich) was used to synthesis HAP-MMT nanocomposites and sodium fluoride, 99.5% (Merck) was used to prepare the fluoride stock solutions.
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3

Heavy Metal Removal via Biocomposite

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Chitosan (degree of deacetylation ≥ 75%, viscosity 20–300 cps), anhydrous calcium chloride granules (7.0 mm, 93.0%), ferric chloride hexahydrate (ACS reagent, 97%), montmorillonite, cupric chloride dihydrate (ACS reagent, ≥ 99.0%) were purchased from Sigma-Aldrich, Mumbai, India. Sodium alginate (pure) from Sisco laboratories, Chennai and carboxymethyl cellulose from Molychem, Mumbai, were obtained. Norfloxacin (C16H18FN3O3, Analytical standard, ≥98%) purchased from Merck, Mumbai. Distilled deionized water (Millipore system) was used in all experiments, and all other chemicals were directly utilized with no additional purification.
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4

Preparation of PVA-Chitosan-MMT Nanocomposite

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PVA (MW 72,000 g/mol) was
obtained from Deajung, Korea. Chitosan (MW range 50,000–190,000
g/mol) and montmorillonite (MMT) were purchased from Sigma-Aldrich,
Korea. Glutaraldehyde was obtained from Panreac Applichem, Spain.
Rutin hydrate was obtained from Crown Chemicals, Pakistan. Ethanol
was obtained from Lab-Scan, Lahore, Pakistan. Quench cream was purchased
from market sources.
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5

Dual Emulsion for PLA/MMT/Trastuzumab NPs

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A double emulsification technique was used to produce the PLA/MMT/TRA NPs. Briefly, 50 mg of PLA (Sigma-Aldrich) were dissolved in 2 mL of dichloromethane (Sigma-Aldrich) and added to 200 µL of PVA (Sigma-Aldrich) solution (0.1% w/v, and 50 mg of Trastuzumab (TRA, Herceptin, Roche Laboratories). This solution was sonicated (UP100H, Hielscher, Teltow, Germany) for two cycles of 30 s at 45 W. Then, 4 mL of aqueous PVA solution (0.7% w/v) and 0.42% clay (MMT; Montmorillonite; Sigma-Aldrich) were added and sonicated (UP100H, Hielscher, Teltow, Germany) for 60 s. The residual organic solvent was evaporated (Rotavapor R114, Buchi, Postfach, Switzerland) under reduced pressure for 1 h. Finally the NPs were recovered by ultra-centrifugation (20,000 rpm) at 25 °C for 20 min (Centrifugal Beckman Coulter J 25, Brea, California, USA). Physicochemical property measurements of freshly synthesized NPs were immediately performed61 (link). Monoclonal antibody entrapment efficacy in PLA/MMT/TRA particles was measured using a BCA assay in parallel62 (link).
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6

Chitosan-Based Nanocomposite Hydrogel

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Acros-Organics company was the supplier of Chitosan (CS) with a molecular weight of 100,000–300,000 (Zeel West Zone 2, Janssen Pharmaceuticalan 3a, B2440, Geel, Belgium). Poly(vinyl alcohol) (PVOH) (low molecular weight i.e., 13,000–23,000, hydrolysis degree 87–89%) was purchased by SIGMA-ALDRICH (Co., 3050 Spruce Street, St. Louis, MO, USA, 314-771-5765). Nanocor Inc. was provided the powder nanoclay (2870 Forbs Avenue, Hoffman Estates, IL, USA). Montmorillonite which contained 1.53% halloysite nanotubes (Al2Si2O5(OH)4∙2H2O, 99.5% clay, 1.68% CaO, 3.35% Fe2O3, 62.9% SiO2, 19.6% Al2O3, and 3.05% MgO) was obtained by Sigma-Aldrich (product 685445, Sigma-Aldrich, St. Louis, MO, USA). The used Thyme Oil (TO) was produced by the Chemco company (Via Achille Grandi, 13–13/A, 42030 Vezzanosul, Crostolo, Italy).
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7

Synthesis and Characterization of Chitosan-PVA Nanocomposites

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Acros-Organics company (Zeel West Zone 2, Janssen Pharmaceuticalan 3a, B2440, Geel, Belgium) was the provider of chitosan with a molecular weight of 100,000–300,000. SIGMA-ALDRICH, Co., 3050 Spruce Street, St. Louis, MO 63103 USA 314-771-5765 was the supplier of poly(vinyl alcohol) (PVOH) with low molecular weight (13,000−23,000) and hydrolysis degree of 87−89%. The same company was also the provider of zinc acetate dihydrate (Zn(CH3COO)2·2H2O), 25% ammonia solution, and montmorillonite (Mt) (code name Nanomer PGV) with a mass density of 2.6 g/cm3 and CEC value of 145 meq/100 g. The last chemical was purchased from Nanocor Inc., 2870 Forbs Avenue Hoffman Estates, IL 60192, IL, United States. Sigma-Aldrich was the supplier of the montmorillonite (product 685445, Sigma-Aldrich, St. Louis, MO, USA) with a chemical composition of 1.53% halloysite nanotubes (Al2Si2O5(OH)4·2H2O, 99.5% clay), 1.68% CaO, 3.35% Fe2O3, 62.9% SiO2, 19.6% Al2O3, and 3.05% MgO.
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8

Acetylcholinesterase Inhibition Assay

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Acetylcholinesterase
(AChE, EC 3.1.1.7, Type VI-S, 254 U/mg from electric eels), acetylthiocholine
chloride (ATCh), chlorpyrifos, carbaryl, kaolinite (Kaol), montmorillonite
(Mt), bentonite (Bent), sepiolite (Sep), hydrogen tetrachloroaurate
(HAuCl4·3H2O), sodium borohydride (NaBH4), 3-aminopropyl triethoxysilane (APTES), 5,5′-dithiobis(2-nitrobenzoic
acid) (DTNB), disodium hydrogen phosphate (Na2HPO4), sodium dihydrogen phosphate (NaH2PO4), sodium
hydroxide (NaOH), potassium chloride (KCl), and potassium ferricyanide
(K3[Fe(CN)6]) were purchased from Sigma-Aldrich.
In addition, 100% acetic acid (CH3COOH) and 99.9% ethanol
(CH3CH2OH) were obtained from QReC Chemical.
Chitosan (CS, average MW = 550 kDa, and
95% acetylation) was obtained from Seafresh Chitosan Co., Ltd., Thailand.
Deionized water was prepared from a Thermo Scientific Barnstead EASY
pure deionization unit. All the chemicals used were of analytical
grade and applied without further treatment.
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9

Characterization of Reservoir Minerals

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Reservoir
minerals quartz-sand, Kaolinite, illite, and montmorillonite were
used in the study. Quartz was collected from Teluk Ramunia in Johor
Bahru, Malaysia. The quartz samples were subsequently washed and air-dried
for 24 h. Next, the air-dried sample was dried at 105 °C for
24 h in an oven. Illite was acquired from Kuala Rompin, Pahang, Malaysia
and used as received. Kaolinite and montmorillonite were purchased
from Sigma-Aldrich (USA). The surface area of the samples was determined
by the BET (Brunauer–Emmett–Teller) method using a Micrometrics
surface analyzer (model: Micrometrics AccuSorb 2100E, USA). Furthermore,
powder X-ray diffraction (XRD) equipment from Smart Lab, Rigaku (USA),
scanning electron microscopy (SEM), and an electron-dispersive X-ray
(EDX) model S0433N-Hitachi were conducted to characterize the proportion
of any minerals present in the samples. In this study, the SEM–EDX
analyses were employed to determine compositions and morphologies
of the different clay minerals.
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10

Characterization of Clay Minerals

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Montmorillonite (Sigma-Aldrich, Japan), hectorite
(Wako, Japan), kaolinite (Fluka, Japan), glycerin (Merck, Germany),
sorbitol (Merck, Germany), formamide (Merck, Germany), and ethylene
glycol (S.D. Fine Chemicals Ltd., India) were purchased and used as
received. Deionized water, unless otherwise noted, was used throughout
the work.
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