AOAC 2018 Methods

(c) 1,3-Dipalmitoyl-2-chloropropanediol.- (TRC, art. D486840, www.trc-canada.com) or equivalent. CAS No. 169471-41-4: PP-2-MCPD, 98% chemical purity. (d) 1,3-Dipalmitoyl-2-chloropropanediol-d5 . (TRC, art. D486842, www.trc-canada.com) or equivalent. CAS No. : PP-2-MCPD-d5, 98% chemical purity, 98% isotopic purity. (e) Glycidyl Palmitate.- (Wako, art. 072-05741, www.wako-chem.co.jp/english/) or equivalent. CAS No. 7501-44-2: Gly-P, 98% purity. (f) Glycidyl Palmitate-d5 .- (TRC, art. G615954, www.trc-canada.com) or equivalent. CAS No. 1794941-80-2: Gly-P-d5, 97% chemical purity, 98% isotopic purity. (g) 2-Chloropropane-1,3-diol.- (art. C379690, www.trc-canada.com) or equivalent. CAS No. 497- 04-1, 98% purity. (h) 3-Chloropropane-1,2-diol .-(art. C379710, www.trc-canada.com) or equivalent. CAS No. 96-24- 2, 98% purity. (i) d5-3-Chloropropane-1,2-diol .- minimum 98 % isotopic purity (art. DLM-4633, www.isotope.com) or equivalent. CAS No. 342611-01-2, 95% chemical purity, 99% isotopic purity. (j) d5-2-Chloropropane-1,3-diol .- (art. C379692, www.trc-canada.com) or equivalent. CAS No. 1216764-05-4, 96% purity. (k) Tetrahydrofuran .- anhydrous, ≥99.9% (Sigma -Aldrich, art. 401757, www.sigmaaldrich.com) or equivalent. CAS No. 109-99-9. (l) Methanol .- HiPerSolv CHROMANORM® Reag. Ph. Eur., gradient grade for HPLC, ≥99.8% (VWR, art. 20864.320, www.vwr.com) or equivalent. CAS No. 67-56-1. (m) n-Heptane .- for analysis EMSURE® Reag. Ph Eur, ≥99% (Merck, art. 104379, www.merckmillipore.com) or equivalent. CAS No. 142-82-5. (n) Acetone .- BAKER ANALYZED® A.C. S. Reagent, ≥99.5% (J.T.Baker, art. 9006 -03, www.avantormaterials.com) or equivalent. CAS No. 67-64-1. (o) Toluene .- for gas chromatography ECD and FID SupraSolv®, ≥99.8% (Merck, art. 108389, www.merckmillipore.com) or equivalent. CAS No. 108-88-3. (p) Sulfuric acid .- ACS reagent, 95.0-98.0%, (Sigma-Aldrich, art. 258105, www.sigmaaldrich.com) or equivalent. CAS No. 7664-93-9. (q) Sodium hydrogen carbonate .- for analysis EMSURE® ACS, Reag. Ph Eur (Merck, art. 106329, www.merckmillipore.com) or equivalent. CAS. No. 144-55-8. (r) Sodium sulfate anhydrous.- for analysis EMSURE® ACS, ISO, Reag. Ph Eur (Merck, art. 106649, www.merckmillipore.com) or equivalent. CAS No. 7757-82-6. (s) Phenylboronic acid .- purum, ≥97.0% (Sigma -Aldrich, art. 78181, www.sigmaaldrich.com) or equivalent. CAS No. 98-80-6. (t) Sodium Bromide .- Alfa Aesar, 87604, 99.99%, metals basis, or equivalent. CAS No. 7647-15-6. (u) Water .- ultra-pure (e.g. Millipore Milli-Q purification system) (v) Ethyl acetate .- PESTINORM® for pesticide residue analysis, 99.7%, (VWR, art. 83660.320, www.vwr.com), or equivalent. CAS No. 141-78-6. (w) Diethyl ether .- AnalaR NORMAPUR® ACS, Reag. Ph. Eur. analytical reagent, 99.7%, (VWR, art. 23811.361, www.vwr.com), or equivalent. CAS No. 60-29-7. (x) N-hexane.- for liquid chromatography LiChrosolv (Merck, art. 104391, www.merckmillipore.com) or equivalent. CAS No. 110-54-3.

D. Reagent Preparation (a) Acid aqueous solution of sodium bromide (sodium bromide 3 mg/mL, sulfuric acid 5% v/v) .- Prepare a concentrated aqueous solution of sodium bromide by dissolving 1 g of sodium