AOAC RI ERP E-Book - DS DF

OMAMAN-38 B: Collaborative Study Protocol Expert Review Panel Use Only September, 2017

HPLC columns.— Two TSK-Gel G2500PWXL columns, 30 cm × 7.8 mm, connected in series. Operate at 80°C. Mobile phase: distilled water at 0.5 mL/min. System must be capable of separating maltose from maltotriose (Figure 2017.xxD). Run time of 60 min to ensure that all materials from the injection are cleared from the column prior to the next injection. Cation and anion exchange guard column (containing de-ionising/ de- salting cartridges).— Cation and anion exchange guard cartridges, H + and CO 2 3- forms respectively. (Bio-Rad Laboratories, Cat. No. 125- 0118, includes one cation and one anion cartridge), with guard column holder (Bio-Rad Labratories, Cat. No. 125-039) to hold the two guard cartridges in series, cation cartridge preceeding anion cartridge). http://www.bio-rad.com/en-jp/sku/1250118-micro-guard-de-ashing- refill-cartridges Guard column (or pre-column).— TSK Gel PWx1 guard column (TOSOH). Detector.— Refractive index (RI); maintained at 50°C. Data integrator or computer.— For peak area measurement. Filters for disposable syringe.— 0.45 µm membrane, 13 mm or 25 mm. Filters for water.— polyvinylidene fluoride, pore size 0.45 µm, 47 mm. Filter apparatus.— To hold 47 mm, 0.45 µm filter, B(a) to filter larger volumes of water.

(u)

(v)

(w)

(x) (y) (z)

(aa) (bb)

Syringes.— 10 mL, disposable, plastic.

(cc) (dd) (ee)

Syringes.— Hamilton 100 µ L, 710SNR syringe. AOAC Research Institute ERP Use Only Rotary evaporator .—Heidolph Laborota 4000 or equivalent. http://www.heidolphna.com (ff) Thermometer .—Capable of measuring to 100°C.

C. Reagents

(a) EtOH 95 % v/v. or Industrial Methylated Spirits (IMS). Industrial Methylated Spirits made up of: EtOH 84.8333 (w%), 85.952 (v%); water 5.6571 (w%), 4.524 (v%); 2-propanol 4.9118 (w%), 5.0000 (v%); methanol 4.5979 (w%),

9