Mar Jorge L Guzmán, Reyes Laura Hinojosa, Rahman G M Mizanur, Kingston H M Skip
Department of Chemistry and Biochemistry, Duquesne University, Pittsburgh, Pennsylvania 15282, USA.
J Agric Food Chem. 2009 Apr 22;57(8):3005-13. doi: 10.1021/jf803598k.
A microwave-assisted enzymatic extraction (MAEE) method was developed for the simultaneous extraction of arsenic (As) and selenium (Se) species in rice products. The total arsenic and selenium content in the enzymatic extracts were determined by inductively coupled plasma mass spectrometry (ICP-MS), while the speciation analysis was performed by ion chromatography coupled to inductively coupled plasma-mass spectrometry (IC-ICP-MS). The main factors affecting the enzymatic extraction process were evaluated in NIST SRM-1568a rice flour. The optimum extraction conditions were 500 mg of sample, 50 mg of protease XIV, and 25 mg of alpha-amylase in aqueous medium during 40 min at 37 degrees C. The extraction recoveries of total As and Se reached 100 +/- 3 and 80 +/- 4%, respectively. The species stability study during the MAEE process did not show transformation of the target species in rice products. The results of As speciation obtained for SRM-1568a were in agreement with previous studies of As speciation performed on the same reference material. The proposed method was applied to the determination of As and Se species in rice and rice-based cereals. Arsenite [As(III)], arsenate [As(V)], dimethylarsinic acid (DMA), and selenomethionine (SeMet) were the predominant species identified in rice products.
开发了一种微波辅助酶提取(MAEE)方法,用于同时提取大米制品中的砷(As)和硒(Se)形态。酶提取物中的总砷和硒含量通过电感耦合等离子体质谱(ICP-MS)测定,而形态分析则通过离子色谱-电感耦合等离子体质谱联用(IC-ICP-MS)进行。在NIST SRM-1568a米粉中评估了影响酶提取过程的主要因素。最佳提取条件为:在水介质中,500 mg样品、50 mg蛋白酶XIV和25 mgα-淀粉酶,于37℃下提取40分钟。总砷和硒的提取回收率分别达到100±3%和80±4%。MAEE过程中的形态稳定性研究表明,大米制品中的目标形态没有发生转化。SRM-1568a的砷形态分析结果与之前对同一参考物质进行的砷形态研究结果一致。所提出的方法应用于大米和大米类谷物中砷和硒形态的测定。亚砷酸盐[As(III)]、砷酸盐[As(V)]、二甲基砷酸(DMA)和硒代蛋氨酸(SeMet)是大米制品中鉴定出的主要形态。