超声辅助提取-高相液相色谱-电感耦合等离子体质谱法测定香菇中6种形态砷化合物

Arsenic Speciation Analysis of Lentinus edodes by Ultrasonic-Assisted Extraction-High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

建立一种同时测定香菇中6种形态砷化合物(亚砷酸根、砷酸根、一甲基砷酸、二甲基砷酸、砷甜菜碱、砷胆碱)的超声辅助提取-高效液相色谱-电感耦合等离子体质谱(high performance liquid chromatography-inductively coupled plasma mass spectrometry,HPLC-ICP-MS)分析方法。选取0.3 mol/L乙酸溶液作为提取剂,超声辅助提取香菇样品中的砷化合物,选用Hamilton PRP X-100阴离子交换柱,25 mmol/L磷酸二氢铵和水作为流动相进行梯度洗脱,经HPLC-ICP-MS进行分离和定量分析。结果表明,在优化实验条件下,6种形态砷化合物在0~50μg/L范围内线性良好,相关系数R^2均在0.998 0以上,检出限为0.31~0.59 μg/L,相对标准偏差为1.6%~3.7%,加标回收率在94.30%~102.75%之间。4种处理方式后的香菇样品的测定结果显示,无机砷是主要的砷化合物,占总砷含量的48.68%~64.25%。方法灵敏度高,前处理简单高效,可以有效地分析香菇样品中不同形态的砷化合物。

The speciation of arsenic in Lentinusedodeswasanalyzed using ultrasonic-assisted extraction（UAE） combined with high performance liquid chromatography-inductively coupled plasma massspectrometry（HPLC-ICP-MS）.Six arsenic compoundswere extracted ultrasonically from the samplesusing 0.3 mol/L acetic acid solution asextraction solvent.The chromatographic separation wasperformed on a Hamiton PRP-X100 anion exchange column using a mixture of 25 mmol/L ammonium dihydrogen phosphate and water asthe mobile phase.Under the optimized conditions,there were good linear relationships in the range of 0–50 μg/L for six arsenic compounds,with correlation coefficients all above 0.998 0.The limit of detection（LODs） of six arsenic species（AsC,AsB,DMA,MMA,As^Ⅲ,and As^Ⅴ） were between 0.31 and 0.59 μg/L.The precision of the method,expressed asrelative standard deviation（RSD）,waslessthan 5%.The recoveriesof AsC,AsB,AsIII,DMA,MMA,and AsV were in the range of 94.30%–102.75%.Speciation analysiscould accurately determine six arsenic speciesin L.edodes.Inorganic arsenic wasthe main speciesin L.edodes,which wasin the range of 48.68%–64.25%.Thismethod wassimple,rapid,sensitive and accurate,and could meet the requirementsfor the quantitative analysisof arsenic speciation in plant materials.