Rodríguez I, Lee H K, Li S F
Department of Chemistry, National University of Singapore, Republic of Singapore.
Electrophoresis. 1999 Jul;20(9):1862-8. doi: 10.1002/(SICI)1522-2683(19990701)20:9<1862::AID-ELPS1862>3.0.CO;2-8.
Extraction conditions by ion-pair solid-phase extraction of biogenic amines from soy sauce samples were studied. The type of surfactant used as ion-pair reagent, the mode of extraction and the pH were factors studied to enhance the extraction efficiency. High recoveries were obtained using dodecylbenzenesulfonic acid as ion-pair reagent. Octanesulfonate and decanesulfonate did not provide satisfactory recoveries. A dynamic ion-pair solid-phase extraction method was also tested for comparison. The extracted amines were derivatized with fluorescein isothiocyanate, separated by micellar electrokinetic chromatography and detected by laser-induced fluorescence (MEKC-LIF). Because of sample clean-up after extraction and the very high number of theoretical plates obtained with the MEKC-LIF method, identification and quantification of biogenic amines in soy sauce samples could be accomplished. Biogenic amines in soy sauce samples could be separated and quantified with detection limits of the order of 0.1 microg/mL, depending on the sample source.
研究了采用离子对固相萃取法从酱油样品中提取生物胺的萃取条件。用作离子对试剂的表面活性剂类型、萃取方式和pH值是为提高萃取效率而研究的因素。使用十二烷基苯磺酸作为离子对试剂可获得较高的回收率。辛烷磺酸盐和癸烷磺酸盐的回收率不理想。还测试了动态离子对固相萃取法以作比较。萃取的胺用异硫氰酸荧光素衍生化，通过胶束电动色谱分离并用激光诱导荧光检测（MEKC-LIF）。由于萃取后样品得到净化，且MEKC-LIF方法获得的理论塔板数非常高，因此可以完成酱油样品中生物胺的鉴定和定量。根据样品来源，酱油样品中的生物胺可被分离和定量，检测限约为0.1μg/mL。
