高效液相色谱-电感耦合等离子体-串联质谱测定水产品中5 种形态砷

建立高效液相色谱-电感耦合等离子体-串联质谱法（high performance liquid chromatography-inductively coupled plasma tandem mass spectrometry，HPLC-ICP-MS/MS）测定水产品中5 种形态砷的检测方法。利用MS/MS模式，以质量转移的方式消除干扰，流动相由10 mmol/L C2H3NaO2、3 mmol/L KNO3、12 mmol/L NaH2PO4等组成，采用梯度洗脱，As7阴离子交换色谱柱分离。结果表明：5 种形态砷可完全分离，三价砷、二甲基砷、一甲基砷、五价砷和砷甜菜碱都具有良好的线性相关系数，检出限依次为0.005 94、0.005 28、0.008 17、0.008 41、0.011 70 mg/kg，满足检测要求；加标回收率为83%～116%，相对标准偏差均小于5%；该方法具有简便快捷、准确度高、分离明显、检测效率高等特点，可对水产品中多种形态砷进行评价分析。

Determination of Five Arsenic Species in Aquatic Products by High Performance Liquid Chromatography-Inductively Coupled Plasma Tandem Mass Spectrometry

In this study, an analytical method for the determination of five arsenic species in aquatic products by high performance liquid chromatography-inductively coupled plasma tandem mass spectrometry (HPLC-ICP-MS/MS) was established. In this method, interference was eliminated by means of mass transfer in the MS/MS mode. The mobile phase consisted of 10 mmol/L C2H3NaO2, 3 mmol/L KNO3, and 12 mmol/L NaH2PO4. Gradient elution was used for chromatographic separation on an As7 anion exchange column. Under these conditions, five arsenic species could be completely separated. The developed method exhibited good linearity for trivalent arsenic, dimethyl arsenic, monomethyl arsenic, pentavalent arsenic and arsenic betaine, and the detection limits were 0.005 94, 0.005 28, 0.008 17, 0.008 41, 0.011 70 mg/kg, respectively, which met the analytical requirements. The spiked recoveries ranged between 83% and 116%, and the precision expressed as relative standard deviation (RSD) was less than 5%. This method had the characteristics of simplicity, rapidity, high accuracy, good separation, and high detection efficiency. It could be used to evaluate and analyze various species of arsenic in aquatic products.