Lancaster F E, Lawrence J F
Food Research Division, Health Protection Branch, Ottawa, Ontario, Canada.
Food Addit Contam. 1992 Mar-Apr;9(2):171-82. doi: 10.1080/02652039209374059.
Utilizing elements of methodology developed previously for food colours, total free and bound non-sulphonated aromatic amines (NSAA) were determined in commercial samples of soft drink beverages and hard candies. Bound amines in the samples were reduced using sodium dithionite, then total NSAA were extracted into chlorofom, transferred to aqueous acid solution and diazotized with sodium nitrite before coupling with 2-naphthol-3,6-disulphonic acid, disodium salt (R-salt). The coloured derivatives were analysed using reversed-phase ion pair high-performance liquid chromatography (HPLC) and an absorbance detector set at 512 nm. Solid phase extraction cartridges were utilized for extraction and clean-up of the food colours present in the sample, and the concentration of each dye was determined quantitatively using HPLC and absorbance detector wavelengths of 426, 516 or 625 nm. Levels of total NSAA were compatible with those observed previously in food colours. Commercial soft drinks were found to contain (expressed in terms of total free plus bound NSAA in the beverage) 0.19-12.6 ng/ml of aniline, 0.83-8.25 ng/ml 1-naphthylamine and 0.62-1.12 ng/ml 2-naphthylamine. Levels of 0.66-9.15 ng/g of aniline and 2.48-10.6 ng/g 1-naphthylamine were found in commercial samples of hard candies. Bound NSAA in hard candies appeared to survive the manufacturing process. Recoveries averaged 96.9% for tartrazine and 89.6-97.2% for the bound amines when hard candies were prepared in the laboratory.
利用先前开发的用于食用色素的方法原理，对软饮料和硬糖的商业样品中的总游离和结合态非磺化芳香胺（NSAA）进行了测定。使用连二亚硫酸钠还原样品中的结合态胺，然后将总NSAA萃取到氯仿中，转移至酸性水溶液中，并用亚硝酸钠进行重氮化，之后与2-萘酚-3,6-二磺酸二钠盐（R盐）偶合。使用反相离子对高效液相色谱（HPLC）和设置在512 nm的吸光检测器对有色衍生物进行分析。利用固相萃取柱对样品中存在的食用色素进行萃取和净化，并使用HPLC和426、516或625 nm的吸光检测器波长对每种染料的浓度进行定量测定。总NSAA的含量与先前在食用色素中观察到的含量相符。发现市售软饮料中（以饮料中总游离加结合态NSAA表示）苯胺含量为0.19 - 12.6 ng/ml，1-萘胺含量为0.83 - 8.25 ng/ml，2-萘胺含量为0.62 - 1.12 ng/ml。在市售硬糖样品中发现苯胺含量为0.66 - 9.15 ng/g，1-萘胺含量为2.48 - 10.6 ng/g。硬糖中的结合态NSAA似乎在制造过程中未被破坏。在实验室制备硬糖时，柠檬黄的回收率平均为96.9%，结合态胺的回收率为89.6 - 97.2%。
