Tsuda T, Nakanishi H, Morita T, Takebayashi J
J Assoc Off Anal Chem. 1985 Sep-Oct;68(5):902-5.
A method was developed for simultaneous gas chromatographic determination of sorbic acid, dehydroacetic acid, and benzoic acid used as preservatives, and succinic acid, fumaric acid, malic acid, and tartaric acid used as acidulants in soft drinks and jams. A sample was dissolved in NH4OH-NH4Cl pH 9 buffer solution, and an aliquot of the solution was passed through a QAE-Sephadex A 25 column. The column was washed with water, and the carboxylic acids were eluted with 0.1N HCl. Sorbic acid, dehydroacetic acid, and benzoic acid were extracted with ethyl ether-petroleum ether (1 + 1), and determined on a 5% DEGS + 1% H3PO4 column. Succinic acid, fumaric acid, malic acid, and tartaric acid in the lower layer were derivatized with N,O-bis(trimethylsilyl)acetamide and trimethylchlorosilane, and determined on a 3% SE-30 column. Recoveries from soft drink and jam samples fortified with 0.1% each of 7 carboxylic acids ranged from 92.4 to 102.6% for preservatives, and from 88.1 to 103.2% for acidulants.
开发了一种气相色谱法,用于同时测定用作防腐剂的山梨酸、脱氢乙酸和苯甲酸,以及用作软饮料和果酱酸味剂的琥珀酸、富马酸、苹果酸和酒石酸。将样品溶解于pH 9的NH4OH-NH4Cl缓冲溶液中,取一份溶液通过QAE-葡聚糖A 25柱。用水洗涤该柱,并用0.1N HCl洗脱羧酸。用乙醚-石油醚(1 + 1)萃取山梨酸、脱氢乙酸和苯甲酸,并在5% DEGS + 1% H3PO4柱上进行测定。下层中的琥珀酸、富马酸、苹果酸和酒石酸用N,O-双(三甲基硅基)乙酰胺和三甲基氯硅烷衍生化,并在3% SE-30柱上进行测定。在添加了0.1%的7种羧酸的软饮料和果酱样品中,防腐剂的回收率为92.4%至102.6%,酸味剂的回收率为88.1%至103.2%。