Senyuva Hamide Z, Gökmen Vural
Ankara Test and Analysis Laboratory, Scientific and Technical Research Council of Turkey, Ankara 06330, Turkey.
Food Addit Contam. 2005 Mar;22(3):214-20. doi: 10.1080/02652030500109834.
An improved analytical method for the determination of acrylamide in coffee is described using liquid chromatography coupled to mass spectrometric detection (LC-MS). A variety of instant, ground and laboratory roasted coffee samples were analysed using this method. The sample preparation entails extraction of acrylamide with methanol, purification with Carrez I and II solutions, evaporation and solvent change to water, and clean-up with an Oasis HLB solid-phase extraction (SPE) cartridge. The chromatographic conditions allowed separation of acrylamide and the remaining matrix co-extractives with accurate and precise quantification of acrylamide during MS detection in SIM mode. Recoveries for the spiking levels of 50, 100, 250 and 500?microg/kg ranged between 99 and 100% with relative standard deviations of less than 2%. The effects of roasting on the formation of acrylamide and colour development were also investigated at 150, 200 and 225 degrees C. Change in the CIE (Commission Internationale de l'Eclairage) a* colour value was found to show a good correlation with the change in acrylamide. CIE a* and acrylamide data was fitted to a non-linear logarithmic function for the estimation of acrylamide level in coffee. Measured acrylamide levels in commercial roasted coffees compared well with the predicted acrylamide levels from the CIE a* values.
描述了一种使用液相色谱-质谱检测(LC-MS)测定咖啡中丙烯酰胺的改进分析方法。使用该方法对各种速溶咖啡、研磨咖啡和实验室烘焙咖啡样品进行了分析。样品制备包括用甲醇萃取丙烯酰胺,用Carrez I和II溶液净化,蒸发并将溶剂换成水,以及用Oasis HLB固相萃取(SPE)柱进行净化。色谱条件允许在SIM模式下的质谱检测过程中分离丙烯酰胺和其余基质共萃取物,并对丙烯酰胺进行准确和精确的定量。50、100、250和500μg/kg加标水平的回收率在99%至100%之间,相对标准偏差小于2%。还研究了在150、200和225℃下烘焙对丙烯酰胺形成和颜色发展的影响。发现CIE(国际照明委员会)a颜色值的变化与丙烯酰胺的变化具有良好的相关性。将CIE a和丙烯酰胺数据拟合到非线性对数函数,以估计咖啡中的丙烯酰胺水平。商业烘焙咖啡中测得的丙烯酰胺水平与根据CIE a*值预测的丙烯酰胺水平比较吻合。