抗坏血酸-磷酸溶液超声提取-高效液相色谱-电感耦合等离子体质谱法快速测定土壤中6种砷形态的含量  

Rapid Determination of 6 Arsenic Species in Soil by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry after Ultrasound Extraction with Ascorbic Acid-Phosphate Solution

作　　者：杨丽婷 隆星星 王艳萍 郭怀兰[2,3] 张垚 YANG Liting;LONG Xingxing;WANG Yanping;GUO Huailan;ZHANG Yao(Biomedical Research Institute,Hubei University of Medicine,Shiyan 442000,China;Center for Environment and Health in Water Source Area of South-to-North Water Diversion,Hubei University of Medicine,Shiyan 442000,China;School of public health,Hubei University of Medicine,Shiyan 442000,China;Application and Products Centre,Thermo Fisher Scientific,Shanghai 200125,China)

机构地区：[1]湖北医药学院生物医药研究院,十堰442000 [2]湖北医药学院南水北调水源地环境与健康研究中心,十堰442000 [3]湖北医药学院公共卫生与健康学院,十堰442000 [4]赛默飞世尔科技(中国)应用中心,上海200125

出　　处：《理化检验（化学分册）》2024年第8期770-774,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家自然科学基金青年项目(41807409)。

摘　　要：为解决高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS)测定土壤中6种砷形态含量时色谱分离时间长以及亚砷酸根[As(Ⅲ)]易转化成砷酸根[As(Ⅴ)]的问题,进行了题示研究。在0.1 g土壤样品中添加体积比1∶1的1.6 mol·L^(-1)磷酸溶液和0.5 mol·L^(-1)抗坏血酸溶液的混合溶液10 mL,常温下超声提取6 h,用水稀释至50 mL,经0.22μm聚醚砜膜过滤,用HPLC-ICP-MS测定滤液中砷甜菜碱(AsB)、As(Ⅲ)、二甲基砷(DMA)、砷胆碱(AsC)、一甲基砷(MMA)和As(Ⅴ)等6种砷形态的含量。在色谱分析中,以Dionex IonPac AG7色谱柱(50 mm×4 mm,10μm)为分析柱和保护柱,不同体积比的3.5 mmol·L^(-1)碳酸铵溶液和100 mmol·L^(-1)碳酸铵溶液的混合溶液为流动相进行梯度洗脱。结果显示:6种砷形态的质量浓度均在一定范围内和峰面积呈线性关系,检出限(3S/N)为0.010~0.050μg·L^(-1);按照标准加入法进行回收试验,回收率为92.0%~110%,测定值的相对标准偏差(n=6)均小于5.0%。方法用于6个实际土壤样品的分析,检出了As(Ⅲ)和As(Ⅴ),检出量分别为0.07~0.15μg·g^(-1)和3.44~8.61μg·g^(-1)。The study mentioned by the title was conducted to solve problems of the long chromatographic separation time as well as arsenite radical[As(Ⅲ)]being easily converted into arsenate[As(V)]for the determination of 6 arsenic species in soil by high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS).The 10 mL of mixed solution of 1.6 mol·L^(-1)phosphoric acid solution and 0.5 mol·L^(-1)ascorbic acid solution at volume ratio of 1∶1 was added into 0.1 g of the soil sample.The mixture was extracted by ultrasound at room temperature for 6 h.The extract was diluted to 50 mL by water,and the solution obtained passed through a 0.22μm polyethersulfone membrane.The 6 arsenic species including arsenobetaine(AsB),As(Ⅲ),dimethyl arsenic(DMA),arsenocholine(AsC),methyl arsenic(MMA)and As(V)in the filtrate was determined by HPLCICP-MS.In chromatographic analysis,the Dionex IonPac AG7 column(50 mm×4 mm,10μm)was used as the stationary phase,and mixed solutions of 3.5 mmol·L^(-1)ammonium carbonate solution and 100 mmol·L^(-1)ammonium carbonate solution at different volume ratios were used as the mobile phase for gradient elution.It was shown that linear relationships between values of the mass concentration and the peak area of the 6 arsenic species were kept in definite ranges,with detection limits(3S/N)in the range of 0.010-0.050μg·L^(-1).Test for recovery was made according to the standard addition method,giving recoveries in the range of 92.0%-110%,and RSDs(n=6)of the determined values were less than 5.0%.The proposed method was used for the analysis of 6 actual soil samples,and As(III)and As(V)were detected,with detection amounts of 0.07-0.15μg·g-1 and 3.44-8.61μg·g-1,respectively.

关 键 词：抗坏血酸 高效液相色谱-电感耦合等离子体质谱法 砷 形态分析 土壤 

分 类 号：O657.63[理学—分析化学]