摘要
为了测定烟草中砷(As)的形态,采用超声溶剂萃取、高效液相色谱(HPLC)与电感耦合等离子体质谱(ICP-MS)联用技术建立了亚砷酸[As(Ⅲ)]、砷酸[As(V)]、二甲基肿酸(DMA)、甲基胂酸(MMA)、砷甜菜碱(AsB)和砷胆碱(AsC)6种形态As的分离分析方法。结果表明:采用HamiltonPRPX-100(250mm×4.1mm,10μm)阴离子交换柱、15mmol/L(NH4)2HPO4(pH6.0)等度洗脱,6种不同形态As在15min内实现了基线分离,线性范围不小于两个数量级,检出限0.44~0.98μg/L,加标回收率85.19%~87.31%,相对标准偏差(RSDs,n=5)2.45%~3.56%。烟草中As含量较低,且部分以低毒的DMA、MMA形态存在;超声溶剂提取能同时提取烟草中的有机As和无机As,较客观地反映样品中As的形态分布。该方法准确、可靠,适合于评价烟草中As的形态,可为烟草的安全性评价提供参考。
In order to determine the chemical species of arsenic (As) in tobacco samples, a method combining ultrasonic solvent extraction and high performance liquid chromatography (HPLC) with inductively coupled plasma-mass spectrometry (ICP-MS) was developed to separate and analyze six species of arsenic, including arsenous acid [As(Ill)], arsenic acid [As(V)], dimethylarsinic acid (DMA), monomethylarsonic acid (MMA), arsenobetaine (AsB), and arsenocholine (AsC). The result showed that the baselines of the six species of arsenic mentioned above were separated within 15 mins by Hamilton PRPX-100 (250×4.1 mm,10 μm) anion exchange column and using 15 mmol/L (NH4)2HPO4 (pH6.0) as the mobile phase. The linear ranges were no less than two orders of magnitude. The detection limit ranged from 0.44 to 0.98μg/L and the recoveries were from 85.19% to 87.31% with the RSD (n=5) of 2.45% to 3.56%. The content of As in tobacco was low, and some arsenic species existed in the forms of DMA and MMA were of lower toxicity. Ultrasonic solvent extraction could extract the organic and inorganic As in tobacco simultaneously and reflect the distribution of As species in tobacco samples objectively. This method is accurate, reliable, and suitable for the speciation analysis of As in tobacco, and can provide a reference for the safety evaluation of tobacco.
出处
《烟草科技》
EI
CAS
北大核心
2013年第6期53-56,共4页
Tobacco Science & Technology
基金
国家烟草专卖局卷烟减害技术重大专项子项目"‘七匹狼’卷烟主流烟气7种成分释放量影响因素研究"(110200902013)