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采用四极杆电感耦合等离子体质谱法测定内脏中镉和铅的方法验证

Method validation for determination of cadmium and lead in offal by means of quadrupole inductively coupled plasma mass spectrometry.

作者信息

D'Ilio Sonia, Petrucci Francesco, D'Amato Marilena, Di Gregorio Marco, Senofonte Oreste, Violante Nicola

机构信息

Department of Environment and Primary Prevention, Istituto Superiore di Sanità, Viale Regina Elena 299, Rome, Italy.

出版信息

J Agric Food Chem. 2008 Dec 24;56(24):11584-8. doi: 10.1021/jf8028623.

Abstract

Offal includes viscera and internal organs that have been removed from butchered animals, that may be either directly eaten or processed for the production of other foodstuff. Such organs are able to accumulate high concentrations of potentially toxic heavy metals posing a risk for human health when ingested. Because high levels of Cd and Pb may produce damages to humans, Commission Regulation no. 1881/2006 and its amendment established maximum levels for those two elements in edible bovine, porcine, and ovine offal. In the present study, a method based on microwave acid-assisted digestion and quadrupole inductively coupled plasma mass spectrometric quantification of Cd and Pb in offal was validated according to the EU common standards. The main parameters evaluated in the validation process were: the detection and the quantification limits (LoD, LoQ), the recovery, the repeatability, the within-laboratory reproducibility, the linearity range, and the standard measurement uncertainty. The results obtained for LoD and LoQ in microg kg(-1) were, respectively, Cd, 1.8 and 5.4; Pb, 5.1 and 15.5; meanwhile, the mean recovery was about 98% for Cd and 103% for Pb. Repeatability was around 5% for Cd and 4% for Pb. The expanded standard measurement uncertainty, expressed as percentage and with a coverage factor of 2, was estimated as follows: Cd, 4.9%; Pb, 8.7%. For both elements, the main contribution was due to the within-laboratory reproducibility of the measurements.

摘要

内脏包括从屠宰动物身上取出的内脏器官,这些内脏器官既可以直接食用,也可以经过加工用于生产其他食品。这类器官能够蓄积高浓度的潜在有毒重金属,摄入后会对人体健康构成风险。由于高含量的镉和铅可能对人体造成损害,欧盟委员会第1881/2006号法规及其修正案规定了这两种元素在可食用牛、猪和羊内脏中的最高限量。在本研究中,根据欧盟通用标准验证了一种基于微波酸辅助消解和四极杆电感耦合等离子体质谱法定量测定内脏中镉和铅的方法。验证过程中评估的主要参数有:检测限和定量限(LoD、LoQ)、回收率、重复性、实验室内再现性、线性范围以及标准测量不确定度。以微克/千克(μg kg⁻¹)为单位得到的LoD和LoQ结果分别为:镉,1.8和5.4;铅,5.1和15.5;同时,镉的平均回收率约为98%,铅的平均回收率约为103%。镉的重复性约为5%,铅的重复性约为4%。以百分比表示且包含因子为2时,扩展标准测量不确定度估计如下:镉,4.9%;铅,8.7%。对于这两种元素,主要贡献来自测量的实验室内再现性。

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