Zhang Yu, Ren Yiping, Zhao Hangmei, Zhang Ying
Department of Food Science and Nutrition, College of Biosystems Engineering and Food Science, Zhejiang University, Hangzhou 310029, Zhejiang Province, PR China.
Anal Chim Acta. 2007 Feb 19;584(2):322-32. doi: 10.1016/j.aca.2006.10.061. Epub 2006 Nov 15.
The present study developed two analytical methods for quantification of acrylamide in complex food matrixes, such as Chinese traditional carbohydrate-rich foods. One is based on derivatization with potassium bromate and potassium bromide without clean-up prior to gas chromatography with micro-electron capture detector (GC-MECD). Alternatively, the underivatized acrylamide was detected by high-performance liquid chromatography coupled to quadrupole tandem mass spectrometry (HPLC-MS/MS) in the positive electrospray ionization mode. For both methods, the Chinese carbohydrate-rich samples were homogenized, defatted with petroleum ether and extracted with aqueous solution of sodium chloride. Recovery rates for acrylamide from spiked Chinese style foods with the spiking level of 50, 500 and 1000 microg kg(-1) were in the range of 79-93% for the GC-MECD including derivatization and 84-97% for the HPLC-MS/MS method. Typical quantification limits of the HPLC-MSMS method were 4 microg kg(-1) for acrylamide. The GC-MECD method achieved quantification limits of 10 microg kg(-1) in Chinese style foods. Thirty-eight Chinese traditional foods purchased from different manufacturers were analyzed and compared with four Western style foods. Acrylamide contaminant was found in all of samples at the concentration up to 771.1 and 734.5 microg kg(-1) detected by the GC and HPLC method, respectively. The concentrations determined with the two different quantitative methods corresponded well with each other. A convenient and fast pretreatment procedure will be optimized in order to satisfy further investigation of hundreds of samples.
本研究开发了两种用于测定复杂食品基质(如中国传统富含碳水化合物的食品)中丙烯酰胺含量的分析方法。一种方法是基于溴酸钾和溴化钾衍生化,在使用微电子捕获检测器的气相色谱分析(GC-MECD)之前无需净化处理。另一种方法是采用高效液相色谱-四极杆串联质谱联用(HPLC-MS/MS)在正电喷雾电离模式下检测未衍生化的丙烯酰胺。对于这两种方法,将富含碳水化合物的中国食品样品进行均质化处理,用石油醚脱脂,并用氯化钠水溶液萃取。对于添加水平为50、500和1000 μg kg⁻¹的加标中式食品,GC-MECD衍生化方法测定丙烯酰胺的回收率在79 - 93%之间,HPLC-MS/MS方法的回收率在84 - 97%之间。HPLC-MS/MS方法测定丙烯酰胺的典型定量限为4 μg kg⁻¹。GC-MECD方法在中国食品中的定量限为10 μg kg⁻¹。分析了从不同制造商购买的38种中国传统食品,并与4种西式食品进行比较。通过GC和HPLC方法分别检测到所有样品中均存在丙烯酰胺污染物,浓度分别高达771.1和734.5 μg kg⁻¹。两种不同定量方法测定的浓度相互吻合良好。为了满足对数百个样品的进一步研究,将优化一种简便快速的预处理程序。