高效液相色谱-电感耦合等离子体质谱法测定栉孔扇贝中6种砷形态化合物

Determination of 6 arsenic species in Chlamys Farreri by high performance liquid chromatography-inductively coupled plasma mass spectrometry

中文关键词:  砷形态  高效液相色谱-电感耦合等离子体质谱法  栉孔扇贝  砷甜菜碱

英文关键词:arsenic speciation  high performance liquid chromatography-inductively coupled plasma mass spectrometry  Chlamys Farreri  arsenobetaine

中文摘要:

      目的 建立高效液相色谱-电感耦合等离子体质谱法(high performance liquid chromatography-inductively coupled plasma mass spectrometry, HPLC-ICP-MS)定量测定栉孔扇贝中6种砷形态的方法。方法 称取均质后的样品1.0 g置于50 mL离心管中, 加入5 mmol/L(NH4)2CO3溶液20 mL, 混匀, 超声提取30 min, 经0.45 μm滤膜过滤。采用DionexIonPac AS-7(250 mm×4.0 mm, 10 μm)色谱柱分离, 流动相为5 mmol/L(NH4)2CO3溶液和200 mmol/L(NH4)2CO3溶液, 然后ICP-MS测定栉孔扇贝中的6种砷形态。结果 市售栉孔扇贝中总砷含量高, 64.8%~86.0%砷元素是以无毒砷甜菜碱的形式存在, 无机砷含量低于国标限量要求。在优化实验条件下, 6种砷形态质量浓度在0~100 μg/L范围内线性良好, 检出限(3 S/N)在0.0002~ 0.0005 mg/kg之间, 定量限在0.001~0.002 mg/kg之间, 加标回收率在80.0%~100.4%之间, RSD在2.02%~5.78%之间。结论 该方法快速、准确、灵敏, 适合测定栉孔扇贝中的主要砷形态化合物。

英文摘要:

      Objective To establish a method for the quantitative determination of 6 species of arsenic in Chlamys Farreri by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS). Methods The homogenized sample of 1.0g was weighed and placed in a 50 mL centrifuge tube. The sample was added with 5 mmol/L(NH4)2CO3 solution of 20 mL, mixed, ultrasonic extracted for 30 min, and filtered through a 0.45 m filter membrane. A DionexIonPac AS-7 (250 mm×4.0 mm, 10 μm) column was used for separation. The mobile phase consisted of 5 mmol/L (NH4)2CO3 and 200 mmol/L (NH4)2CO3. Six arsenic species in Chlamys Farreri were determined by ICP-MS. Results The total arsenic content in commercial scallop Chlamys Farreri was high, 64.8%–86.0% arsenic element existing in the form of non-toxic arsenic betaine, and the inorganic arsenic content was lower than the national standard limit. Under the optimized experimental conditions, the concentration of the 6 arsenic species was linear in the range of 0–100 μg/L, the detection limits were between 0.0002–0.0005 mg/kg, the quantitative limits were between 0.001–0.002 mg/kg, the recovery rates were between 80.0%–100.4%, and the RSD were between 2.02%~5.78%. Conclusion This method is rapid, accurate and sensitive, and is suitable for the determination of major arsenic species in Chlamys Farreri.