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4 protocols using uplc grade acetonitrile

1

Comprehensive Pesticide Analysis Protocol

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High purity pesticide (>98%) standards of ethephon, glufosinate, fosetyl, phosphonic acid, glyphosate, and hydroxyethyl phosphonic acid (HEPA) were purchased from LGC‐Dr. Ehrenstorfer (Augsburg, Germany), N‐acetyl‐AMPA, N‐acetyl‐glufosinate, N‐acetyl‐glyphosate, and 3‐methylphosphinicopropionic acid (MPPA) from Toronto Research Chemicals, TRC (North York, Canada), aminomethyl phosphonic acid (AMPA) was purchased from Sigma–Aldrich (Steinheim, Germany) and bromide, chlorate, and perchlorate were obtained from Inorganic Ventures (Christiansburg, Virginia, USA). Isotope–labeled internal standards, AMPA 13C 15N, ethephon D4, fosetyl–aluminum D15, HEPA D4, glufosinate D3 hydrochloride, N‐acetyl‐glufosinate D3, MPPA D3, glyphosate 1,2‐13C2, 15N, and N‐acetyl‐glyphosate D3 were purchased from LGC‐Dr. Ehrenstorfer was obtained from Toronto Research Chemicals. Phosphonic acid‐18O3, 18O3‐chlorate, and 18O4‐perchlorate were supplied by the EURL‐SRM in Stuttgart, Germany. HPLC‐grade water from a Water Purification System of Millipore (Burlington, MA, USA) was used. Formic acid was purchased from VWR (Lutterworth, United Kingdom) and trifluoroacetic acid (TFA) was obtained from Merck (Darmstadt, Germany). UPLC‐grade acetonitrile and LC‐grade methanol were supplied by Biosolve (Dieuze, France) and Merck (Darmstadt, Germany), respectively.
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2

UPLC Solvent Preparation for Analysis

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Ultra-performance liquid chromatography (UPLC)-grade acetonitrile, isopropanol, methanol, ethyl acetate and purified water were purchased from Biosolve B.V. (Valkenswaard, the Netherlands). Acetic acid, ammonium hydroxide, ammonium acetate and 2-proponal were acquired from Sigma-Aldrich (Zwijndrecht, the Netherlands). Sodium dihydrogen phosphate dihydrate, sodium hydrogen phosphate and sodium acetate were obtained from Merck (Darmstadt, Germany).
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3

Alkalization of Cocoa Powder Extraction

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Commercial cocoa powder produced from Forastero cocoa nibs with 10-12% (w/w) fat was supplied by Cargill (Schiphol, Netherlands). Analytical grade NaOH (98%) for alkalization was purchased from Chem-Lab NV (Zedelgem, Belgium) and demineralized water was purified using an Elix type 2 pure water system 20 from Merck Millipore (Overijse, Belgium). UPLC-grade acetonitrile, methanol, formic acid and ammonium formate were purchased from Biosolve (Valkenswaard, The Netherlands), while n-hexane (≥ 97%), acetone (99.8%) and acetic acid (99.8%) were purchased from Acros Organics (Geel, Belgium). Analytical standards were purchased from Extrasynthese (Lyon, France), Sigma-Aldrich (Bornem, Belgium), Santa Cruz Biotechnology (Heidelberg, Germany), or Carl Roth (Karlsruhe, Germany). All other chemicals were of the highest grade commercially available.
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4

Chocolate Characterization Protocol

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White chocolate callets (lot No. 191070202), ruby RB1 chocolate callets (lot No. 183340601, 191880601) , milk chocolate callets (Power 41) (lot No. 190700202 ) and dark chocolate callets (Recipe N⁰ 70-30-38, lot No. 183170102, 190870201 ) , all from Callebaut, were purchased in a Belgian baking shop. UPLC-grade acetonitrile, methanol, formic acid and ammonium formate were purchased from Biosolve (Valkenswaard, The Netherlands). HPLC-grade acetone was obtained from Acros Organics (Geel, Belgium), and HPLC-grade n-hexane and methanol came from Fisher Scientific (Loughborough, UK). Ultrapure water was generated with a Direct Pure Up system of Rephile. Amberlite XAD-7HP was supplied by Acros Organics (Geel, Belgium). Analytical standards were purchased from Extrasynthese (Lyon, France), Sigma-Aldrich (Bornem, Belgium), Santa Cruz Biotechnology (Heidelberg, Germany), or Carl Roth (Karlsruhe, Germany).
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