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12 protocols using milli q direct 8 water purification system

1

Preparation of MBSH and Acetic Acid Solutions

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Acetonitrile (HPLC grade), p-toluene sulfonyl hydrazide (4-methylbenzenesulfonohydrazide/MBSH, 97%), acetic acid (100%), and formaldehyde (37% w/v in water, containing 10–15% methanol) were all purchased from Merck KGaA (Darmstadt, Germany). Formic acid (99–100%) was purchased from VWR (Radnor, Pennsylvania, USA). The UHQ water (≤18 MΩ) was supplied in house by a Milli-Q direct 8 water purification system (Millipore, Burlington, Massachusetts, USA).
A MBSH solution in Acetonitrile (2 mg/mL) was prepared by dissolving 100 mg of MBSH in Acetonitrile to a volume of 50 mL. An acetic acid solution (200 μg/mL) was prepared by dissolving 10 μL of acetic acid in 50 mL of water. Methylthioninium chloride (MTC) samples 1–6 were provided by TauRx Therapeutics Ltd (Aberdeen, United Kingdom).
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2

Kaolinite Dispersion Preparation for SFG and Electrokinetic Analyses

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Materials. Polygloss® 90 kaolinite sample (325 mesh, with a median size of 44 microns based on dynamic light scattering, KaMin Performance Minerals) was used for the preparation of kaolinite dispersions used for both SFG and electrokinetic measurements. NaCl (99.99%, trace metals basis, Alfa Aesar) was used for the preparation of kaolinite dispersions. NaOH pellets (99.99% semiconductor grade, trace metals basis, Sigma-Aldrich), Ca(OH)2 prepared by slaking highcalcium quick lime (≥ 90% calcium oxide) (Graymont Inc., Calgary, Alberta, Canada)) with water, and HCl (34-37%, trace metal grade, Fisher Scientific) were used to prepare the titrant for pH adjustments. KCl (99.999%, trace metals basis, Acros Organics) was used to calibrate the SurPASS conductivity meter. Methanol (HPLC grade, Fisher Chemical), sulfuric acid (95.0 -98.0%, Caledon Laboratories) and hydrogen peroxide (30% w/w in H2O, Sigma-Aldrich) were mixed in a 3:1 ratio and used for piranha cleaning of silica hemispheres and plates. All materials were used without further purification. Ultrapure water (18.2 MΩ•cm) was used from a Milli-Q Direct 8 Water Purification System (Millipore).
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3

Cochineal Powder Dye Extraction Protocol

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Cochineal powder was obtained from Panreac (Barcelona, Spain). Chromotrope FB (carmoisine, CAS no. 3567-69-9) (dye content 50%) was purchased from Sigma-Aldrich (Steinheim, Germany). Sodium tetraborate decahydrate (CAS no. 1303-96-4) and methanol (CAS no. 67-56-7) (gradient grade for liquid chromatography 8/33 LiChrosolv®) were obtained from Merck (Darmstadt, Germany). Hydrochloric acid (37%, CAS no. 7647-01-0) was supplied by VWR International (Radnor, Pennsylvania, USA).
The Milli-Q ® Direct 8 water purification system from Millipore (Bedford, MA, USA) was used to obtain deionised water.
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4

Lipid Formulation Preparation and Characterization

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2-oleoyl-1-palmitoyl-sn-glycero-3-phosphocholine (POPC) (phosphatidylcholine, ≥99%; Mw 760.08 g/mol), 1-palmitoyl-sn-glycero-3-phosphocholine (Lyso-PC) (lysophosphatidylcholine, ≥99%; Mw 495.63 g/mol), free cholesterol (≥99%; Mw 386.65 g/mol), oleic acid (reagent grade, ≥99%; Mw 282.46 g/mol), 1-monooleoyl-rac-glycerol (monoolein, C18:1,-cis-9, Mw 356.54 g/mol), taurocholic acid sodium salt hydrate (NaTC) (≥95%; Mw 537.68 g/mol) ), cholecalciferol (>98%; Mw 384.64 g/mol; melting point 84.5°C; solubility in water: 10 -4 -10 -5 mg/mL; logP 7.5) and retinyl palmitate (>93.5%; Mw 524.86 g/mol; melting point 28.5°C; logP 13.6) were purchased from Sigma-Aldrich (Saint-Quentin-Fallavier, France). Chloroform and methanol (99% pure) were analytical grade reagents from Merck (Germany). Ethanol (99.9%), n-hexane, Chloroform, acetonitrile, dichloromethane and methanol were HPLC grade reagents from Carlo Erba Reagent (Peypin, France). Ultrapure water was produced by a Milli-Q ® Direct 8 Water Purification System (Millipore, Molsheim, France). Prior to all surface tension, and surface pressure experiments, all glassware was soaked for an hour in a freshly prepared hot TFD4 (Franklab, Guyancourt, France) detergent solution (15% v/v), and then thoroughly rinsed with ultrapure water. Physico-chemical properties of D 3 and RP were retrieved from PubChem (https://pubchem.ncbi.nlm.nih.gov/).
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5

Cochineal Powder Characterization Protocol

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Cochineal powder was obtained from Panreac (Barcelona, Spain). Erythrosine B (CAS no. 16423-68-0, for microscopy), methanol (CAS no. 67-56-7) (gradient grade for liquid chromatography LiChrosolv®) and sodium tetraborate decahydrate (CAS no. 1303-96-4) were purchased from Merck (Darmstadt, Germany). Hydrochloric acid (37%, CAS no. 7647-01-0) was from VWR International (Radnor, Pennsylvania, USA).
Deionised water was obtained by using the Milli-Q ® Direct 8 water purification system from Millipore (Bedford, MA, USA).
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6

ICP-MS and ICP-OES Calibration Standards

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For the calibration step of ICP-MS, various standards were used, including the ICP IV multi-element standard (1000 mg·L−1; each element) (Merck, New York, NY, USA) and single standards (1000 mg·L−1; each element): As, Sb, Se, Mo and V (Sigma-Aldrich, New York, NY, USA) and Hg (Merck, USA). Additionally, as internal standards, Sc, Rh, Tb and Ge in supra-pure 1% HNO3 (Merck, New York, NY, USA) and deionized water collected from the Milli-Q Direct 8 Water Purification System (Merck Millipore, New York, NY, USA) were used for all solution preparation. For the calibration of ICP-OES, the single standards (1000 mg·L−1; each element) of Ca, Na, Mg and K were used (Sigma-Aldrich, New York, NY, USA).
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7

ICP-MS Elemental Analysis Protocol

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The ICP IV multi-element standard (Merck KGaA, Darmstadt, Germany) and single standards—As, Sb, Se, Mo and V (Merck KGaA, Darmstadt, Germany), Hg (Merck KGaA, Darmstadt, Germany)—were used for the calibration of ICP-MS. Sc, Rh, Tb and Ge in supra-pure 1% HNO3 (Merck KGaA, Darmstadt, Germany) were used as internal standards, and deionized water obtained from the Milli-Q Direct 8 Water Purification System (Merck-Millipore, Molsheim, France) was used for sample dilution.
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8

Calibration of ICP-MS and ICP-OES Analyses

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For calibration of ICP-MS the ICP IV multi element standard was used (Merck, New York, NY, USA) and single standards: As, Sb, Se, Mo and V (Sigma-Aldrich, New York, NY, USA), Hg (Merck, USA). Moreover, as an internal standards Sc, Rh, Tb and Ge in supra pure 1% HNO3 (Merck, New York, NY, USA) and deionized water obtained from the Milli-Q Direct 8 Water Purification System (Merck Millipore, New York, NY, USA) were used for sample (pre)treatment and sample dilution. For calibration of ICP-OES the Sigma Aldrich (USA) stock solution containing 1000 mg L−1 of Ca, Mg, and K were used to prepare calibration standards. The accuracy of the analyses was verified by means of certified reference materials: trace metals ICP—sample 1 and trace metals ICP—sample 2. The retrieval of the selected elements in both CRMs ranged from 97% to 105%. At the same time, water and matrix calibration standards were compared (in 1.2% C2H5OH) and no significant differences were found in the obtained values of the analytical signals from the both standards type.
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9

Formulation and Characterization of Antacid Hydrogel

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Met HCl was purchased from Farmhispania, S.A. (Barcelona, Spain). Alginic acid sodium salt from brown algae with medium viscosity (Sod ALG), sodium chloride, and hydrochloric acid fuming 37% were obtained from Sigma-Aldrich (St. Louis, MO, USA). Natrosol™ 250 hydroxyethylcellulose (HEC) HHX grade was purchased from Ashland (Covington, KY, USA). Calcium carbonate and sodium carbonate (USP grade) were obtained from Daejung (Siheung, Korea). Gaviscon Double Action was purchased from Oxy Reckitt Benckiser (Seoul, Korea). Purified water was prepared using a Milli-Q® Direct 8 Water Purification System from EMD Millipore (Darmstadt, Germany). HPLC grade solvents were used for high-performance liquid chromatography.
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10

Comprehensive Compound Acquisition Protocol

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The following were obtained from Sigma-Aldrich (St. Louis, MO, USA): l-Glutamate, l-cysteic acid, 4-(2-hydroxyethyl)-1-piperazineethanesulfonic acid (HEPES), acetonitrile, boric acid, phenobarbital, sucrose, calcium chloride, potassium chloride, magnesium chloride, DMSO, verapamil hydrochloride, carbamazepine, and 4-aminopyridine. From the Tokyo Chemical Industry (Tokyo, Japan), the following was purchased: 4-fluoro-7-nitrobenzofurazan (NBD-F). The following were provided by Cyclolab Ltd (Budapest, Hungary): β-cyclodextrin and 6-monodeoxy-6-mono(3-hydroxy) propylamino -β-cyclodextrin hydrochloride. The following were obtained from Tocris Bioscience (Bristol, UK): dl-threo-β-benzyloxyaspartic acid (dl-TBOA), tetrodotoxin, and ω-conotoxin MVIIC. The following were purchased from Reanal (Hungary, Budapest): sodium chloride and D-glucose. Fetal bovine serum was obtained from Biosera (Nuaille, France). Lidocaine hydrochloride was provided by Egis Pharmaceutical Plc. (Budapest, Hungary). Tolperisone and pregabalin were received as kind gifts from Meditop Pharmaceuticals Ltd. (Budapest, Hungary). Ultrapure water from MilliQ Direct 8 water purification system (Merck, Darmstadt, Germany) was used for all experiments. All compounds were stored and handled as described in the product information sheets.
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