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Determination of Rh, Pd and Pt in urine samples using a pre-concentration sequential injection analysis system coupled to a quadrupole-inductively coupled plasma-mass spectrometer

机译:使用与四极杆电感耦合等离子体质谱仪耦合的预浓缩顺序注射分析系统测定尿液样品中的Rh,Pd和Pt

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The proposed flow system was developed in order to minimize the drawbacks related to the PGEs determination by quadrupole-inductively coupled plasma-mass spectrometry (Q-ICP-MS). It was intended not only to lower the limits of detection (LODs) but also to eliminate the interferences originating from some atomic and molecular ions produced in the argon plasma. This was accomplished by means of an on-line sample clean-up/pre-concentration step, using a chelating resin (Metalfix~(TM)Chelamine~(TM)) in which Rh, Pd and Pt were preferably retained when compared with the interfering species. The results obtained by using the developed flow system in the analysis of urine samples are presented. With a sampling rate of 9 samples h~(-1) (i.e., 27 determinations) and a sample consumption of ca. 10 mL, the developed flow system allowed linear calibration plots up to 100 ngL~(-1) with detection limits of 1.2 ng L~(-1) (Rh), 0.4ngL~(-1) (Pd) and 0.9ngL~(-1) (Pt). Repeatability studies showed good precision (R.S.D.%, n = 5): 3.7% (Rh); 2.6% (Pd) and 2.4% (Pt), for 10 ngL~(-1); 2.4% (Rh); 1.4% (Pd) and 1.9% (Pt), for 50 ng L~(-1); and 1.3% (Rh); 0.58% (Pd) and 0.62% (Pt), for 100 ng L~(-1). By spiking human urine samples, recovery tests were performed, and the values obtained ranged between 89% and 105% (Rh); 90% and 104% (Pd); and 93% and 105% (Pt).
机译:开发提出的流量系统是为了最大程度地减少与通过四极电感耦合等离子体质谱法(Q-ICP-MS)测定PGE有关的缺点。它不仅旨在降低检测限(LOD),而且旨在消除源自氩等离子体中产生的某些原子和分子离子的干扰。这是通过使用螯合树脂(MetalfixTMChelamineTM)进行的在线样品净化/预浓缩步骤来实现的,其中与Rh相比,Rh,Pd和Pt优选保留在其中。干扰物种。介绍了通过使用发达的流动系统分析尿液样品获得的结果。以9个样本的采样率h〜(-1)(即27个测定)和大约消耗的样本量10 mL,开发的流量系统可进行高达100 ngL〜(-1)的线性校准图,检测限为1.2 ng L〜(-1)(Rh),0.4ngL〜(-1)(Pd)和0.9ngL〜 (-1)(点)。重复性研究显示出良好的精度(R.S.D.%,n = 5):3.7%(Rh); 10 ngL〜(-1)为2.6%(Pd)和2.4%(Pt); 2.4%(相对湿度); 50 ng L〜(-1)为1.4%(Pd)和1.9%(Pt);和1.3%(Rh); 100 ng L〜(-1)为0.58%(Pd)和0.62%(Pt)。通过加标人类尿液样本,进行了恢复测试,所得值在89%至105%(Rh)之间; 90%和104%(钯);和93%和105%(Pt)。

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