Takatsuki Satoshi, Nemoto Satoru, Sasaki Kumiko, Maitani Tamio
National Institute of Health Sciences: 1-18-1, Kamiyoga, Setagaya-ku, Tokyo 158-8501, Japan.
Shokuhin Eiseigaku Zasshi. 2003 Apr;44(2):89-95. doi: 10.3358/shokueishi.44.89.
An LC/MS method was developed for the determination of acrylamide (AA) in processed or cooked foods. AA was extracted with a mixture of water and acetone from homogenized food samples after the addition of 13C-labeled acrylamide (AA-1-(13)C) as an internal standard. The extract was concentrated, washed with dichloromethane for defatting, and cleaned up on Bond Elut C18, PSA and ACCUCAT cartridge-columns, and then AA was determined by LC/MS in the selected ion recording (SIR) mode. For the LC/MS analysis, four LC columns were connected in-line and the flow of the mobile phase was switched according to a time-program. Monitoring ions for AA were m/z 72 and 55, and those for AA-1-(13)C were m/z 73 and 56. AA and AA-1-(13)C were determined without interference from the matrices in all samples. The recoveries of AA from potato chips, corn snack, pretzel and roasted tea spiked at the level of 500 ng/g of AA were 99.5-101.0% with standard deviations (SD) in the range from 0.3 to 1.6%. The limits of detection and quantification of the developed method were 9 and 30 ng/g for AA in samples, respectively. The method was applied to the analysis of AA in various processed or cooked food samples purchased from retail markets. High levels of AA were found in potato chips and French-fried potato (467-3,544 ng/g). Fried and sugar-coated dough cakes (karinto) contained 374 and 1,895 ng/g. Corn snacks contained 117-535 ng/g of AA. Roasted foods (such as roasted sesame seed, roasted barley (mugi-cha), roasted tea (hoji-cha), coffee beans and curry powder) contained 116-567 ng/g of AA. Foods made from fish, egg and meat contained lower levels of AA than the plant-based foods. Foods containing much water showed a tendency to have low levels of AA compared with dry foods. The proposed method was applicable to the analysis of AA in variety of processed foods.
建立了一种液相色谱/质谱(LC/MS)方法,用于测定加工食品或烹饪食品中的丙烯酰胺(AA)。在加入13C标记的丙烯酰胺(AA-1-(13)C)作为内标后,用含有水和丙酮的混合液从匀浆的食品样品中提取AA。提取物经浓缩后,用二氯甲烷洗涤以脱脂,并在Bond Elut C18、PSA和ACCUCAT柱上进行净化处理,然后采用LC/MS在选择离子记录(SIR)模式下测定AA。进行LC/MS分析时,将四根液相色谱柱串联连接,并根据时间程序切换流动相的流速。AA的监测离子为m/z 72和55,AA-1-(13)C的监测离子为m/z 73和56。所有样品中的AA和AA-1-(13)C在测定时均不受基质干扰。在薯片、玉米零食、椒盐脆饼和焙茶中添加浓度为500 ng/g的AA,其回收率为99.5%-101.0%,标准偏差(SD)在0.3%-1.6%范围内。所建立方法对样品中AA的检测限和定量限分别为9 ng/g和30 ng/g。该方法应用于从零售市场购买的各种加工食品或烹饪食品样品中AA的分析。结果发现,薯片和炸薯条中AA含量较高(467-3544 ng/g)。油炸裹糖面饼(karinto)中AA含量分别为374 ng/g和1895 ng/g。玉米零食中AA含量为117-535 ng/g。焙烤食品(如焙烤芝麻、焙烤大麦(麦茶)、焙茶(焙茶)、咖啡豆和咖喱粉)中AA含量为116-567 ng/g。鱼、蛋和肉制成的食品中AA含量低于植物性食品。与干货相比,含水量高的食品中AA含量往往较低。所提出的方法适用于各种加工食品中AA的分析。