García Falcón M S, González Amigo S, Lage Yusty M A, López de Alda Villaizán M J, Simal Lozano J
Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Pharmacy, University of Santiago de Compostela, Spain.
J Chromatogr A. 1996 Nov 15;753(2):207-15. doi: 10.1016/s0021-9673(96)00522-5.
We developed a procedure for trace enrichment of benzo[a]pyrene (BP) in extracts of smoked food products, and an HPLC-fluorescence detection (FL) method for determination of BP in the enriched extracts. The procedure consists in extraction/sonication of the lyophilized product in hexane, clean-up of the hexane extract by passage through a Sep-Pak Silica Plus cartridge and, subsequently, by partitioning between hexane and dimethyl sulphoxide, and concentration of the BP using a Sep-Pak C18 Plus cartridge. HPLC-FL and quantification limits were 0.049 microgram/l in acetonitrile (< 0.0067 microgram/kg of smoked food) and 0.089 microgram/l in acetonitrile (< 0.012 microgram/kg), respectively. Recovery (94.1%) and RSD (< 8.65%) were satisfactory. When applied to 15 types of sausage, mean BP content was 0.022 microgram/kg, and all but two samples (both treated with wood smoke) had BP contents below the 0.03 microgram/kg limit imposed in EU legislation for smoking-flavour agents.
我们开发了一种用于烟熏食品提取物中苯并[a]芘（BP）痕量富集的方法，以及一种用于测定富集提取物中BP的高效液相色谱 - 荧光检测（FL）方法。该方法包括将冻干产品在己烷中进行萃取/超声处理，通过Sep-Pak Silica Plus柱净化己烷提取物，随后通过己烷和二甲基亚砜之间的分配，并使用Sep-Pak C18 Plus柱浓缩BP。高效液相色谱 - 荧光检测法的检测限和定量限在乙腈中分别为0.049微克/升（<0.0067微克/千克烟熏食品）和0.089微克/升（<0.012微克/千克）。回收率（94.1%）和相对标准偏差（<8.65%）令人满意。将该方法应用于15种香肠时，BP平均含量为0.022微克/千克，除两个样品（均用木烟熏制）外，所有样品的BP含量均低于欧盟法规对烟熏风味剂规定的0.03微克/千克限值。
