HPLC-ICP-MS测定泽泻、金银花、鸡血藤中可溶性价态砷及残留限度

Speciations of Soluble Arsenic and the Limit Standard in Alismatis Rhizome, Lonicerae Japonicae Flos and Spatholobi Caulis by HPLC-ICP-MS

关键词:  高效液相色谱-电感耦合等离子质谱  金银花  泽泻  鸡血藤  砷  形态  残留限度

Key words:  HPLC-ICP-MS  Alismatis Rhizome  Lonicerae Japonicae Flos  Spatholobi Caulis  arsenic  speciation  limit standard

摘要:

目的 建立高效液相色谱-电感耦合等离子质谱(HPLC-ICP-MS)测定方法，分析金银花、泽泻、鸡血藤中4种不同价态砷，评估泽泻、金银花、鸡血藤中4种价态砷的残留情况，为制定相关残留限度提供依据。方法 采用0.05 mol·L^-1 EDTA溶液超声提取样品中可溶性砷，采用HPLC-ICP-MS分析样品中可溶性砷的形态。结果 As(Ⅲ)、DMA、MMA、As(Ⅴ)在5~200 μg·L^-1内线性良好，平均回收率(n=9)为105.1％~108.4％，方法检测限为0.01 mg·kg^-1。泽泻检出少量As(Ⅲ)、As(Ⅴ)，金银花检出少量As(Ⅲ)、DMA、As(Ⅴ)，鸡血藤则均未检出As(Ⅲ)、DMA、MMA、As(Ⅴ)。结论 该方法操作简便、结果准确、重复性好，能满足4种不同价态砷的残留限度分析。

Abstract:

OBJECTIVE To establish a method for determination of the soluble arsenic in Alismatis Rhizome, Lonicerae Japonicae Flos and Spatholobi Caulis by HPLC-ICP-MS. To evaluate the residual of soluble arsenic and provide the basis for the formulation of soluble arsenic residues. METHODS The samples were extracted by 0.05 mol·L^-1 EDTA with ultrasonic treatment, then detected by HPLC-ICP-MS. RESULTS Concentration of As(Ⅲ) , DMA, MMA and As(Ⅴ) in the range of 5-200 μg·L^-1 showed good linear relationship, the average recovery (n=9) were in 108.4%-105.1%, and the detection limit of the method was 0.01 mg·kg^-1. Small amounts of As (Ⅲ), As (Ⅴ) were detected in Alismatis Rhizome. Small amounts of As (Ⅲ), DMA, As (Ⅴ) were detected in Lonicerae japonicae flos. None was detected in Spatholobi Caulis. CONCLUSION The method is simple, accurate, and reproducible, it can be used for analysing the residual limit of As(Ⅲ) , DMA, MMA and As(Ⅴ).