A simple, rapid and sensitive solid phase microextraction method was used for the speciation of inorganic antimony (Sb) by using a novel synthesized polymeric material in micropipette tip of syringe system. In present methodology, the specie of Sb (III) made hydrophobic complex with diethyl dithiocarbamate (DDTC) at pH 5.5 and subsequently adsorbed on polystyrene oleic acid imidazole polymer (POIP), whereas Sb(V) did not made complex and adsorbed on the polymer, remained in aqueous solutions. The strategy of multivariate was carried out to screen out the different variables and assessed the optimum values of their experimental values for the extraction efficiency of analyte. Then the analyte was sorbed on the polymer in micropipette tip of syringe system was quantitatively eluted by different types of acids at different levels for 2–6 aspirating/dispensing cycles. The extracted Sb(III) ions with modifiers were directed into the graphite furnace atomic absorption spectrometry for analysis. The limit of detection (LOD), limit of quantification (LOQ) and preconcentration factor (PF) for Sb(III) was found to be 6 ng L⁻¹, 20 ng L⁻¹ and 100. The RSD value was found to be 4.2%. The standard addition method and certified reference materials were checked for accuracy and validity of method. The developed method was effectively applied for the determination of total and inorganic species of Sb(III) and Sb(V) in different types of water samples, whereas only total Sb was determined in acid digested soil, Tuna fish, rice, spinach, black tea, mixed fruit juice and ice tea samples.

一种简单，快速，灵敏的固相微萃取方法，通过在注射器系统的微量移液器吸头中使用新型合成聚合物材料，用于无机锑（Sb）的形态分析。在目前的方法中，Sb（III）的物种在pH 5.5下与二硫代氨基甲酸二乙酯（DDTC）形成疏水复合物，随后被吸附在聚苯乙烯油酸咪唑聚合物（POIP）上，而Sb（V）没有形成复合物并被吸附在聚合物上保留在水溶液中。进行多变量策略以筛选出不同的变量，并评估其实验值的最佳值以提高分析物的提取效率。然后将分析物吸附在注射器系统微量移液器吸头上的聚合物上，并通过不同类型的酸以不同的浓度定量洗脱2-6次抽吸/分配循环。将提取的具有改性剂的Sb（III）离子导入石墨炉原子吸收光谱法进行分析。发现Sb（III）的检出限（LOD），定量限（LOQ）和预浓缩因子（PF）为6 ng L^-1，20 ng L ^-1和100。RSD值为4.2％。检查标准添加方法和经认证的参考材料的准确性和有效性。所开发的方法有效地用于测定不同类型水样中总和无机形态的锑（III）和锑（V），而在酸消化的土壤，金枪鱼，水稻，菠菜，黑色中仅测定了总锑。茶，混合果汁和冰茶样品。