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建立和验证了一种用感应耦合等离子体质谱法测定牛、马和家禽肝脏中 Cd、Pb 和 As 的方法。

Development and validation of a method for Cd, Pb and As analysis in bovine, equine and poultry liver by inductively coupled plasma mass spectrometry.

机构信息

Ministry of Agriculture, Livestock and Supply - National Agricultural Laboratory, Pedro Leopoldo, MG, Brazil.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2012;29(4):609-16. doi: 10.1080/19440049.2011.608381. Epub 2011 Oct 14.

Abstract

A method for the determination of As, Cd and Pb in bovine, equine and poultry liver by ICP-MS was developed and validated. Samples were digested in a microwave oven using a 10% HNO(3) solution. A set of experiments was made according to a central composite design (CCD) for optimisation of the plasma argon flow, nebuliser argon flow and radiofrequency power applied to the plasma. During the validation, Rh and Ru were evaluated as internal standards and, after validation, the best was Rh for Pb and Cd analysis, but for As better results were obtained without an internal standard. The method allowed As, Cd and Pb determination with a 3.3% HNO(3) solution for the calibration curves ranging from 0 to 40 µg l(-1) for As and from 0 to 20 µg l(-1) for Cd and Pb. The recovery values obtained showed averages of 100%, 106% and 96% for As, Cd and Pb, respectively. Limits of quantification obtained were 85 µg kg(-1) for As, 6.5 µg kg(-1) for Cd and 12.5 µg kg(-1) for Pb. Repeatability and within-laboratory reproducibility were evaluated through the indicators HORRAT(r) and HORRAT(R), and the results were less than 0.30. The method is simple, fast and showed adequate precision and accuracy for the determination of As, Cd and Pb in bovine, equine and poultry liver. The precision, recovery, uncertainties, and limits of detection and quantification for each analyte were in accordance to European Union Commission Regulation 2007/333/EC.

摘要

建立并验证了用 ICP-MS 测定牛、马和家禽肝脏中砷、镉和铅的方法。采用 10%硝酸溶液,在微波消解仪中消解样品。根据中心组合设计(CCD)进行了一组实验,以优化等离子体中的氩气流、雾化器氩气流和射频功率。在验证过程中,评估了 Rh 和 Ru 作为内标物,验证后,对于 Pb 和 Cd 分析,最好使用 Rh,但对于 As 分析,不使用内标物则能获得更好的结果。该方法允许使用 3.3% HNO3 溶液测定校准曲线范围为 0 至 40μg l(-1)的 As 和 0 至 20μg l(-1)的 Cd 和 Pb。获得的回收率平均值分别为 As 的 100%、Cd 的 106%和 Pb 的 96%。获得的定量限分别为 As 的 85μg kg(-1)、Cd 的 6.5μg kg(-1)和 Pb 的 12.5μg kg(-1)。通过 HORRAT(r)和 HORRAT(R)指标评估重复性和实验室内部再现性,结果小于 0.30。该方法简单、快速,对于测定牛、马和家禽肝脏中的 As、Cd 和 Pb 具有足够的精密度和准确度。每个分析物的精密度、回收率、不确定度以及检测限和定量限均符合欧盟委员会 2007/333/EC 法规。

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