序贯提取-高效液相色谱-电感耦合等离子体质谱法测定栉孔扇贝裙边中砷组分

Determination of arsenic components in the skirt of Chlamys farreri by sequential extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometry

中文关键词:  栉孔扇贝  砷形态  扇贝裙边  序贯提取  高效液相色谱-电感耦合等离子体质谱法

英文关键词:Chlamys farreri  arsenic species  scallop skirts  sequential extraction  high performance liquid chromatography-inductively coupled plasma mass spectrometry

中文摘要:

      目的 建立序贯提取-高效液相色谱-电感耦合等离子体质谱法(high performance liquid chromatography-inductively coupled plasma mass spectrometry, HPLC-ICP-MS)测定栉孔扇贝(Chlamys farreri)裙边中砷组分。方法 以超纯水、甲醇及二氯甲烷-甲醇溶液为提取液, 采用序贯涡旋提取法, 提取扇贝裙边中砷, 并划分为水提取砷、非水提取砷及未提取砷3种组分。采用HPLC-ICP-MS砷形态检测法定性定量分析6类水提取已知砷：砷酸、亚砷酸、一甲基胂、二甲基胂、砷甜菜碱、砷胆碱, 采用ICP-MS总砷检测法定量分析总砷、水提取未知砷、非水提取砷及未提取砷。结果 市售栉孔扇贝裙边中总砷含量高, 水提取已知砷、水提取未知砷、非水提砷及未提取砷分别占24.5%、26.8%、25.4%及23.3%, 无机砷含量符合国家限量要求。优化条件下, 6种砷形态在0~100 μg/kg范围内线性关系良好, 检出限为0.014~2.366 μg/kg, 定量限为0.050~3.090 μg/kg, 加标回收率在78.1%~116.2%之间, 相对标准偏差(relative standard deviations, RSDs)在1.1%~10.1%之间。结论 本研究建立的砷组分分析方法精密度高、灵敏度高、砷提取效率高, 适用于扇贝裙边中砷组分的分析, 可为扇贝裙边的安全性评价提供理论依据。

英文摘要:

      Objective To establish a method for the determination of arsenic components in the skirt of Chlamys farreri by sequential extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS). Methods Using ultrapure water, methanol and dichloromethane-methanol solution as extraction solutions, the arsenic in scallop skirts was extracted by sequential vortex extraction and was divided into 3 groups: Water-extracted arsenic, non-water-extracted arsenic and unextracted arsenic. The HPLC-ICP-MS arsenic speciation detection method was used to qualitatively and quantitatively analyze the 6 kinds of water-extracted known arsenic: Arsenate, arsenite, monomethylarsonate, dimethylarsonate, arsenobetaine, arsenocholine, total arsenic, water-extracted unknown arsenic, non-water-extracted arsenic and unextracted arsenic were quantitatively analyzed by ICP-MS total arsenic detection method. Results The total arsenic content in the skirt of commercially available scallops was high, water-extracted known arsenic, water-extracted unknown arsenic, non-water extracted arsenic and unextracted arsenic accounted for 24.5%, 26.8%, 25.4% and 23.3%, respectively, and the content of inorganic arsenic met the national limit requirements. Under the optimized conditions, the 6 kinds of arsenic species had good linear relationships in the range of 0?100 μg/kg, the limits of detection were between 0.014?2.366 μg/kg, the limits of quantification were between 0.050?3.090 μg/kg, the recoveries were between 78.1%?116.2%, and the relative standard deviations (RSDs) were between 1.1%?10.1%. Conclusion The arsenic composition analysis method established in this study has high precision, high sensitivity and high arsenic extraction efficiency, which is suitable for the analysis of arsenic components in scallop skirts and can provide a theoretical basis for the safety evaluation of scallop skirts.