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Determination of Lead in Dietary Supplements by High-Resolution Continuum-Source Graphite Furnace Atomic Absorption Spectrometry with Direct Solid Sampling
Journal of Food Composition and Analysis ( IF 4.0 ) Pub Date : 2020-03-01 , DOI: 10.1016/j.jfca.2019.103360
Gabriela Camera Leal , Patricia Mattiazzi , Franciele Rovasi , Thaís Dal Molin , Denise Bohrer , Paulo Cícero do Nascimento , Leandro M. de Carvalho , Carine Viana

Abstract A method has been developed for the determination of lead (Pb) in dietary supplements using direct solid sampling and high-resolution continuum source graphite furnace atomic absorption spectrometry. The lead concentration was determined in 74 food supplements. The zirconium (Zr) coated platform, and chemical modifiers [Pd(NO3)2 and Mg(NO3)2] were applied. Mass aliquots between 0.8 and 1.0 mg were weighed and directly inserted into the graphite furnace. The precision (expressed as RSD) was lower than 5%, and a detection limit of 2.16 pg was obtained at the 283.306 nm resonance line. The limit of quantification was 7.2 pg. The Pb recuperation in the standard reference material, Bitter Orange-Containing Solid Oral Form NIST SRM 3260, was 116% of the certified value. The contents of Pb in the dietary supplement samples varied in the 0.04–25.3 μg/day range. Two samples had results above that allowed by American Pharmacopoeia for inorganic analysis in food supplements.

中文翻译:

采用高分辨率连续源石墨炉原子吸收光谱法和直接固体取样测定膳食补充剂中的铅

摘要 开发了一种使用直接固体取样和高分辨率连续源石墨炉原子吸收光谱法测定膳食补充剂中铅 (Pb) 的方法。在 74 种食品补充剂中测定了铅浓度。应用了锆 (Zr) 涂层平台和化学改性剂 [Pd(NO3)2 和 Mg(NO3)2]。将 0.8 至 1.0 毫克的质量等分试样称重并直接放入石墨炉中。精密度(以 RSD 表示)低于 5%,在 283.306 nm 共振线处的检出限为 2.16 pg。定量限为 7.2 pg。标准参考物质(含苦橙的固体口服形式 NIST SRM 3260)中的 Pb 回收率为认证值的 116%。膳食补充剂样品中铅的含量在 0.04-25 之间变化。3 μg/天范围。两个样品的结果高于美国药典允许的食品补充剂无机分析结果。
更新日期:2020-03-01
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