Page 272 - Analytical method for food addtives

180 Analytical methods for food additives

Reference 7 8 Reference 3 2

Detection FID at 370 ºC FID at 300 ºC Detection Mobile phase Fluorescence Acetonitrile–water at em 412 nm, (85:15, v/v), 1.5 ex 365 nm mL/min, 20 µL injection 210 nm 2 mM H 3 PO 4 – 1.5 % acetonitrile at 1 mL/min

Method conditions Di(2-ethylhexyl)adipate (DEHA) Column: HP-5MS 0.25 µm film. Temperature programmed 70–280 ºC. Carrier gas: helium. Split injector 1:25, 2 µL injection Column: CP-sil 5CB (50 m × mm, 0.12 µm film). 0.32 Temperature programmed 130–290 ºC. Carrier gas: helium. 0.3 µL injection. Column TSK-Gel, octadecyl-silan

g of packaging material was Soxhlet extracted with chloroform–methanol transferred to 50 mL vol flask and made up to volume with chloroform– methanol. 1 mL transferred to vials for Total adipate: sample saponified with alkali and extracted with ethyl acetate, evaporated and silylated. Free adipate: aqueous extraction, then ext

Sample preparation 1 (2:1), 50 mL for 6 h. Extracts GC–MS analysis silylated with 9-anthryldiazomethane

Matrix Packaging materials Starch Matrix Urine Ice lollies

Table 14.1 cont’d Method GC–MS GC (b) Method HPLC Ion-exclusion chromatography