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2 protocols using titrisol solutions

1

Synthesis and Characterization of Cabotegravir

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Cabotegravir,
its related substances and cabotegravir degradation products were
synthesized/isolated in Lek (Mengeš, Slovenia).8 (link),23 Methanol (MeOH) and acetonitrile (ACN), both gradient grade were
obtained from J.T. Baker now part of Avantor (Radnor, PA, USA). Analytical
grade formic acid, glacial acetic acid, ammonium acetate, hydrochloric
acid (HCl), and sodium hydroxide (NaOH) both Titrisol solutions were
obtained from Merck KGaA (Darmstadt, Germany). Ammonium formate was
obtained from Honeywell (Charlotte, NC, USA). Ultrapure water was
obtained by a Milli-Q system from Merck Millipore (Burlington, MA,
USA).
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2

Cocaine and Metabolite Analysis Protocol

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Stock solutions at 1 mg mL -1 of BZE in MeOH and cocaine base were provided by Sigma-Aldrich (Saint-Quentin-Fallavier, France). The working solutions at 1 µg mL -1 were obtained by dilution of the stock solution (1 mg mL -1 ) in HPLC-grade ACN (Carlo Erba, Val-de-Reuil, France). These solutions were stored at -20°C. MeOH, EtOH, and isooctane were purchased from Carlo Erba. Acetic acid and anhydrous ACN were provided by Sigma-Aldrich. 1 M NaOH and 0.1 M HCl were obtained using deionized water (Milli-Q purification system, Millipore, Molsheim, France) and Titrisol solutions from Merck (Darmstadt, Germany). MAA, TRIM, and 3-(trimethoxysilyl)propyl methacrylate (γ-MAPS) were purchased from Sigma-Aldrich. Azo-N,N'-diisobutyronitrile (AIBN) was purchased from Acros Organics (Noisy-le-Grand, France). MAA was distilled under vacuum in order to remove inhibitors and stored at -20°C. TRIM, AIBN, and γ-MAPS were of satisfactory purity so they were used without further purification. Fused-silica capillaries with a UV transparent fluorocarbon polymer coating (PTFE-coated silica capillaries, 100 µm i.d. x 375 µm outer diameter (o.d.)) were purchased from Polymicro Technologies (Photon Lines, Saint Germain-en-Laye, France).
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