Arkansas Regional Laboratory, Office of Regulatory Affairs, United States Food and Drug Administration (FDA), 3900 NCTR Road, Jefferson, Arkansas 72079, United States.
J Agric Food Chem. 2015 Apr 1;63(12):3153-60. doi: 10.1021/acs.jafc.5b00446. Epub 2015 Mar 19.
We report an analytical methodology for the quantification of common arsenic species in rice and rice cereal using capillary electrophoresis coupled with inductively coupled plasma mass spectrometry (CE-ICPMS). An enzyme (i.e., α-amylase)-assisted water-phase microwave extraction procedure was used to extract four common arsenic species, including dimethylarsinic acid (DMA), monomethylarsonic acid (MMA), arsenite [As(III)], and arsenate [As(V)] from the rice matrices. The addition of the enzyme α-amylase during the extraction process was necessary to reduce the sample viscosity, which subsequently increased the injection volume and enhanced the signal response. o-Arsanilic acid (o-ASA) was added to the sample solution as a mobility marker and internal standard. The obtained repeatability [i.e., relative standard deviation (RSD %)] of the four arsenic analytes of interest was less than 1.23% for elution time and 2.91% for peak area. The detection limits were determined to be 0.15-0.27 ng g(-1). Rice standard reference materials SRM 1568b and CRM 7503-a were used to validate this method. The quantitative concentrations of each organic arsenic and summed inorganic arsenic were found within 5% difference of the certified values of the two reference materials.
我们报告了一种使用毛细管电泳结合电感耦合等离子体质谱(CE-ICPMS)定量大米和米谷类中常见砷形态的分析方法。采用酶(即α-淀粉酶)辅助水相微波提取程序,从大米基质中提取四种常见的砷形态,包括二甲基砷酸(DMA)、一甲基砷酸(MMA)、亚砷酸盐[As(III)]和砷酸盐[As(V)]。在提取过程中添加酶α-淀粉酶是必要的,以降低样品的粘度,从而增加进样量并增强信号响应。邻苯二甲酸氧砷酸(o-ASA)被添加到样品溶液中作为迁移率标记物和内标。四种感兴趣的砷分析物的重复性[即洗脱时间的相对标准偏差(RSD %)]小于 1.23%,峰面积的重复性小于 2.91%。检测限确定为 0.15-0.27ng g(-1)。使用标准参考物质 SRM 1568b 和 CRM 7503-a 验证了该方法。两种参考物质的认证值之间存在 5%差异,定量浓度的每种有机砷和总无机砷均在该范围内。