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首页> 外文期刊>International journal of environmental analytical chemistry >Microwave-assisted solid phase extraction prior to ICP-MS determination of Pd and Pt in environmental and biological samples
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Microwave-assisted solid phase extraction prior to ICP-MS determination of Pd and Pt in environmental and biological samples

机译：ICP-MS测定环境和生物样品中的Pd和Pt之前，采用微波辅助固相萃取

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摘要

A sensitive and selective microwave-assisted solid phase extraction procedure coupled to inductively coupled plasma-mass spectrometry (ICP-MS) is proposed for palladium (Pd) and platinum (Pt) quantification in environmental and biological samples. Pd and Pt were quantitatively retained on commercial thioureido propyl functionalised silica gel packed inside a home-made glass microcolumn, and later eluted with 0.5% thiourea solution under microwave irradiation, followed by ICP-MS determination. The main variables affecting the procedural stages (i.e., sorption and desorption) and ICP-MS determination were optimised. The best conditions found were: (a) sorption: sample acidity, 1 M HC1; sample flow rate, 3 mL min~(-1); (b) desorption: microwave radiation, power 800 W; eluent concentration, 0.5% thiourea; eluent flow rate, 0.5 mL min~(-1); (c) ICP-MS determination: nebuliser feeding, free aspiration (0.3 mLmin~(-1)); internal standard, Rh (5 ugL~(-1)). Analyte recoveries were higher than 90% and concentration factors up to 90 and 92 were achieved for Pd and Pt, respectively. Depending on the conditions, the methodological limits of detection were down to 0.2 ngL~(-1) for both analytes and repeatability, expressed as RSD%, varied between 1.3 and 11.0%. A method selectivity evaluation showed that most of the ICP-MS interferents were either quantitatively separated or more than 86% eliminated, except for Cu (elimination efficiency around 30%). Finally, the method was successfully used to determine Pd in certified reference materials (i.e. human urine and serum) and Pd and Pt in PM_(10) airborne particulate matter fractions.
机译：提出了一种灵敏的，选择性的微波辅助固相萃取方法与电感耦合等离子体质谱法（ICP-MS），用于环境和生物样品中的钯（Pd）和铂（Pt）定量。将Pd和Pt定量保留在包装在自制玻璃微柱中的商品硫脲基丙基官能化硅胶上，然后在微波辐射下用0.5％硫脲溶液洗脱，然后进行ICP-MS测定。优化了影响程序阶段（即吸附和解吸）和ICP-MS测定的主要变量。发现的最佳条件是：（a）吸附：样品酸度，1 M HCl；样品流速，3 mL min〜（-1）; （b）解吸：微波辐射，功率800 W；洗脱液浓度：0.5％硫脲；洗脱液流速，0.5 mL min〜（-1）; （c）ICP-MS测定：雾化器进料，自由抽吸（0.3 mLmin〜（-1））；内标Rh（5 ugL〜（-1））。 Pd和Pt的分析物回收率高于90％，浓缩系数分别达到90和92。根据条件，两种分析物的检测方法限均低至0.2 ngL〜（-1），重复性以RSD％表示，介于1.3和11.0％之间。方法的选择性评估表明，除铜（消除效率约为30％）外，大多数ICP-MS干扰物都被定量分离或去除了86％以上。最后，该方法已成功用于测定认证参考物质（即人尿和血清）中的Pd和PM_（10）空气传播颗粒物组分中的Pd和Pt。

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