Pensabene J W, Fiddler W
U.S. Department of Agriculture, Eastern Regional Research Center, Philadelphia, PA 19118.
J Assoc Off Anal Chem. 1990 Mar-Apr;73(2):226-30.
A rapid, sensitive, and accurate solid-phase extraction method was developed for the measurement of 10 N-nitrosoamino acids (NAAs) in cured meat products. In the procedure, the comminuted meat was mixed with sulfamic acid and Celite, and then added to a glass column containing anhydrous sodium sulfate. The column was washed with pentane, and the NAAs were eluted with ethyl acetate. The eluate was concentrated, then derivatized with diazomethane followed by acetic anhydride-pyridine reagent. The NAA methyl esters and their acylated hydroxy derivatives were separated by gas chromatography on a DB-5 fused silica capillary column and quantitated with a thermal energy analyzer, a chemiluminescence detector specific for nitric oxide derived from the thermal denitrosation of nitrosamines. Recovery of 10 of the NAAs exceeded 75% at the 10 ppb level. The method is applicable to a wide range of cured meat products.
开发了一种快速、灵敏且准确的固相萃取方法,用于测定腌肉产品中的10种N-亚硝基氨基酸(NAA)。在该方法中,将粉碎的肉与氨基磺酸和硅藻土混合,然后加入装有无水硫酸钠的玻璃柱中。用戊烷冲洗柱子,并用乙酸乙酯洗脱NAA。将洗脱液浓缩,然后用重氮甲烷衍生化,接着用乙酸酐-吡啶试剂衍生化。NAA甲酯及其酰化羟基衍生物在DB-5熔融石英毛细管柱上通过气相色谱分离,并用热能分析仪(一种对亚硝胺热脱亚硝化产生的一氧化氮具有特异性的化学发光检测器)进行定量。在10 ppb水平下,10种NAA的回收率超过75%。该方法适用于多种腌肉产品。