Viberg Peter, Nilsson Staffan, Skog Kerstin
Department of Food Technology, Engineering and Nutrition, Lund University, POB 124, 22100, Lund, Sweden.
Anal Bioanal Chem. 2004 Apr;378(7):1729-34. doi: 10.1007/s00216-003-2480-2. Epub 2004 Jan 28.
A miniaturised technique to analyse and detect heterocyclic aromatic amines (HAs) using micro solid-phase extraction ( microSPE) coupled on-line (in-capillary) to capillary electrophoresis (CE) separation with nanospray (nESI) mass spectrometry (MS) detection has been developed. HAs are mutagenic and carcinogenic compounds formed at low levels in protein-rich food during cooking. Due to the low concentrations of HAs and the high complexity of the matrix in which they exist, sensitive and selective analytical methods are required for quantification. microSPE was performed on a packed bed of C(18 )particles inside the CE capillary, which minimised the dead volume. The on-line coupling of SPE, CE and nESI-MS reduced the time for extraction and identification to less than half an hour, which will allow for screening of several samples per day. The new technique provides short analysis time, low sample and solvent consumption, and HAs in standard solutions were easily detected at 12-17 fmol injections, and in spiked urine samples at 750-810 fmol injections.
已开发出一种小型化技术，该技术使用微固相萃取（microSPE）在线（毛细管内）与毛细管电泳（CE）分离联用，并通过纳米喷雾（nESI）质谱（MS）检测来分析和检测杂环芳香胺（HAs）。HAs是在烹饪富含蛋白质的食物过程中低水平形成的致突变和致癌化合物。由于HAs浓度低且其存在的基质高度复杂，因此需要灵敏且具选择性的分析方法进行定量。微固相萃取在CE毛细管内的C(18)颗粒填充床上进行，这将死体积降至最低。固相萃取、毛细管电泳和纳米喷雾质谱的在线联用将提取和鉴定时间缩短至不到半小时，这使得每天能够筛查多个样品。这项新技术分析时间短、样品和溶剂消耗低，在标准溶液中，12 - 17飞摩尔进样量时即可轻松检测到HAs，在加标尿样中，750 - 810飞摩尔进样量时可检测到HAs。
