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7 protocols using methanol meoh

1

Analytical Reagent Purification Protocol

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Desethylatrazine (DEA), desisopropylatrazine, simazine, cyanazine, ATZ, propazine (PPZ), TER, MAA, ethylene glycol dimethacrylate (EGDMA), and 2,2′‐azobis‐2‐methylbutyronitrile (AIMN) were supplied by Sigma‐Aldrich (Madrid, Spain). HEMA was purchased from Merck (Darmstadt, Germany). ACN and methanol (MeOH) were from Scharlab (Barcelona, Spain). AIMN was recrystallized in MeOH and EGDMA and MAA were freed from stabilizers by distillation under reduced pressure prior to use. Purified water was obtained from a Milli‐Q purification system purchased from Millipore (Madrid, Spain). All other chemicals were of analytical reagent grade and used as received.
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2

HPLC Analysis of Potato Glycoalkaloids

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The HPLC-grade solvents such as methanol (MeOH) and ethanol (EtOH) were obtained from Scharlab (Barcelona, Spain), and acetonitrile (ACN) was obtained from Fisher Chemical (Madrid, Spain). Monosodium phosphate (NaH2PO4) and disodium phosphate (Na2HPO4) were purchased from Panreac (Barcelona, Spain). Ultrapure deionized water with a resistance of 18.2 MΩ cm was obtained by a Milli-Q system (Billerca, MA, USA). Nylon syringe filters (0.45 μm, 13 mm) were purchased from Scharlab (Barcelona, Spain). For standard solutions preparation, α-solanine (>99%) and α-chaconine (>99%), purchased from Phytolab (Madrid, Spain), were used. Individual stock standard solutions of α-solanine and α-chaconine were prepared at a concentration of 200 μg/mL in MeOH and stored at −20 °C. The calibration standards were prepared at the appropriate concentrations (1, 2.5, 5, 10, 25, 50, and 100 mg/L for both analytes) by serial dilution of the stock solutions in MeOH. The prepared solutions were stored in the dark at a temperature of −20 °C.
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3

Synthesis and Characterization of Novel Polyurethanes

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(R)-(+)-limonene (LM), hexamethylene diisocyanate (HDI), dibutyltin dilaurate (DBTDL), and sodium tetraphenylborate (NaBPh4) were obtained from Sigma Aldrich (Saint Louis, MO, USA). Squalene (SQ) and 1,8-diazabicyclo(5.4.0)undec-7-ene (DBU) were obtained from Alfa Aesar (Thermo Fisher, Kandel, Germany). Thioacetic acid (TAA) and 2,2-dimethoxy-2-phenylacetophenone (DMPA) were obtained from Acros Organics (Thermo Fisher Scientific, Geel, Belgium). Anhydrous magnesium sulfate (MgSO4) was obtained from (Thermo Fisher Scientific, Geel, Belgium). Sodium hydroxide (NaOH), hydrochloric acid (HCl), chloroform (CHCl3), and methanol (MeOH) were obtained from Scharlab (Barcelona, Spain). All products were used as received. BGDBU, which is a base generator, was synthesized from DBU and sodium tetraphenyl borate according to a reported methodology [24 (link)].
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4

Synthesis of Photosensitive Polymers

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Methyl methacrylate (MMA) (99%),
(2-acetoacetoxy)ethyl methacrylate (AEMA) (95%), 2.2′-azo(2-methylpropionitrile)
(AIBN) (≥98%), p-carboxybenzenesulfon-azide
(p-CBSA) (97%), triethylamine (Et3N) (>99%), HPS (98%), 1,1-dimethyl-2,5-bis(4-(azidomethyl)phenyl)-3,4-diphenylsilole
(Silole-N3) (96%), ethyl acetate
(EtOAc) (anhydrous, 99.8%), diethyl ether (Et2O) (ACS reagent, anhydrous,
>99.0%), dichloromethane (CH2Cl2) (anhydrous, ≥99.8%),
and deuterated chloroform (CDCl3) (99.96 atom % D, containing 0.03% (v/v) tetramethylsilane) were
purchased from Sigma-Aldrich and used, unless specified, as received.
2-Cyanoprop-2-yl-dithiobenzoate (≥97%) was purchased from Strem
Chemicals. Methanol (MeOH) (synthesis grade) and THF (HPLC grade) were purchased from Scharlab. AIBN was recrystallized from methanol. MMA was purified
by distillation before use. AEMA was purified by passing
through alumina.
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5

LC-MS System Validation Protocol

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The LC–MS grade formic acid and acetonitrile (ACN) used for the mobile phases’ preparation were purchased from Fisher Scientific (Pittsburgh, PA, USA) and Scharlab, S.L. (Barcelona, Spain), respectively. The methanol (MeOH) used in the sample and reagent solution preparation was obtained from Scharlab, S.L. (Barcelona, Spain). In addition, ultra-high-purity water, obtained from tap water pre-treated by Elix reverse osmosis and a Milli-Q system from Millipore (Bedford, MA, USA), was used for mobile phase, reagent solutions, and sample preparation.
Standard reagents used to assess the proper LC–MS system operation were from different manufacturers: paracetamol, cholic acid, (±) verapamil hydrochloride, simvastatin, reserpine, and leucine enkephalin acetate salt hydrate were provided by Sigma-Aldrich (Steinheim, Germany); caffeine and salicylic acid were supplied by Alfa Aesar (Karlsruhe, Germany) and Fluka Analytical (Bucharest, Romania), respectively. Finally, sodium fluvastatin was kindly supplied by Novartis (Basel, Switzerland). A system suitability test solution (SST) was prepared with the nine compounds at a final concentration of 100 ng/mL in MeOH:H2O 2:1 (v/v); this solvent composition was chosen as this is similar to the final solution (supernatant) of plasma samples.
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6

Targeted LC-MS/MS Quantification of Olive Phenolics

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LC grade reagents and solvents were used in this research. Ammonium fluoride from Fisher Scientific (Hampton, NH, USA) was used as the ionizing agent. Methanol (MeOH) from Scharlab (Barcelona, Spain) and deionized water (18 mΩ • cm) from a Millipore Milli-Q water purification system (Merck Millipore, Bedford, MA, USA) were used for the preparation of chromatographic mobile phases.
Hydroxytyrosol and tyrosol were purchased from Extrasynthese (Genay, France), whereas secoiridoid derivatives oleacein and oleocanthal were acquired from Phytolab (Vestenbergsgreuth, Germany). On the other hand, oleuropein aglycone and ligstroside aglycone (both as monoaldehyde closed isomers) were purchased from TRC (Ontario, Canada). Syringaldehyde from Sigma-Aldrich (St. Louis, MO, USA) was used as an internal standard (IS) to control the LC-MS/MS performance.
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7

Targeted Analysis of Perfluorinated Compounds

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The target analytes included two perfluorosulfonates which were PFHxS and PFOS and five perfluorocarboxylates which included PFHxA, PFHpA, PFOA, PFNA and PFDA. Internal Standards (I.S.) in methanol included 13 C 2 -PFHxA, 13 C 4 -PFHpA, 13 C 8 -PFOA, 13 C 5 -PFNA, 13 C 6 -PFDA, 18 O 2 -PFHxS and 13 C 8 -PFOS. A list with abbreviations of the nonlabelled and labelled standards is shown in Table S1 of the Supporting information (SI).
The analytical standards and labelled standards were provided as a mixture in methanol by Prof. De Voogt and his team and had originally been procured by Campro Scientific, Veenendaal, The Netherlands. Methanol (MeOH) of LC-MS grade was obtained from Scharlab, while ammonium acetate (AcNH 4 : 77.08 g/mol; 98%) and sodium thiosulfate pentahydrate (Na 2 S 2 O 3 •5H 2 O: 248.18 g/mol; N 99.5%) were obtained from Sigma-Aldrich (Steinheim, Germany). Ultra-pure water having a conductivity of 18 MΩ/cm was prepared using the Elga Purelab Classic purification system.
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