Staruszkiewicz W F, Bond J F
J Assoc Off Anal Chem. 1981 May;64(3):584-91.
A GLC procedure for the quantitative determination of the diamines putrescine and cadaverine has been developed, using their perfluoropropionyl derivatives. The amines were extracted from foods with methanol; an interval standard, hexanediamine, was added and a dry residue of their hydrochloride salts was prepared. The salts were derivatized with perfluoropropionic anhydride by heating for 30 min at 50 degrees C. The reaction mixture was separated on an alumina column to remove excess reagent, and the derivatives were eluted with a solution of 30% ethyl acetate in toluene. GLC separations were performed on a 3% OV-225 column held at 180 degrees C. The retention times were 4.3, 5.7, and 7.0 min for the derivatives for putrescine, cadaverine, and the internal standard, respectively. Less than 1 microgram diamine/g tissue could be quantitated, using either an electron capture detector or a nitrogen-specific detector. The procedure was applied to cheese and a variety of fishery products. An increase in the diamines correlated with the presence of decomposition in some of the products. A collaborative study of the method is planned.
已开发出一种气相色谱法，用于定量测定二胺腐胺和尸胺，该方法使用它们的全氟丙酰衍生物。用甲醇从食品中提取胺类；加入内标己二胺，并制备其盐酸盐的干残渣。将盐与全氟丙酸酐在50℃下加热30分钟进行衍生化。反应混合物在氧化铝柱上分离以除去过量试剂，衍生物用30%乙酸乙酯的甲苯溶液洗脱。在180℃的3% OV - 225柱上进行气相色谱分离。腐胺、尸胺和内标的衍生物的保留时间分别为4.3、5.7和7.0分钟。使用电子捕获检测器或氮特异性检测器可定量低至每克组织低于1微克的二胺。该方法应用于奶酪和各种渔业产品。二胺含量的增加与某些产品中分解的存在相关。计划对该方法进行协同研究。
