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首页> 美国卫生研究院文献>other >Sequential coprecipitation and matrix removal for determination ofcadmium impurities from multivitamin supplements by inductively coupled plasmamass spectrometry and method validation by isotope dilution analysis of SRM 3280multivitamin/multielement tablets
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Sequential coprecipitation and matrix removal for determination ofcadmium impurities from multivitamin supplements by inductively coupled plasmamass spectrometry and method validation by isotope dilution analysis of SRM 3280multivitamin/multielement tablets

机译：顺序共沉淀和基质去除法测定电感耦合血浆中多种维生素补充剂中的镉杂质SRM 3280的同位素稀释分析进行质谱分析和方法验证多种维生素/多种元素片剂

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In this paper, we examined three different sequential coprecipitation schemes based on Mg(OH)2 and CaF2 precipitation using triethylamine (TEA) and hydrofluoric acid (HF), respectively, for determination of cadmium (Cd) impurities from multivitamin/mineral (MVM) supplements by isotope dilution (ID) inductively coupled plasma mass spectrometry (ICP-MS). The schemes involved three-step coprecipitation with either TEA alone or in combination with HF and are designated as Scheme 1 (TEA-TEA-TEA), Scheme 2 (TEA-HF-TEA) and Scheme 3 (HF-TEA-TEA) according to the addition sequence of each reagent. Experiments were carried out with MVM solutions spiked with 60 μg L−1 Cd from a multielement standard solution. All schemes provided quantitative separation of Cd from MVM matrix. Scheme 1 was the least effective in removal of interfering concomitant elements, molybdenum (Mo) and tin (Sn). Scheme 2 performed better for Sn, but failed in eliminating Mo. Scheme 3 was the most effective in eliminating both Mo and Sn. Mo levels in test MVM solutions reduced from 4.3 μg mL−1 to as low as 0.014 μg mL−1 while that for Sn decreased from 0.5 μg mL−1 to 0.018 μg mL−1allowing interference-free determination of Cd to be achieved. Salt-matrix dueto Mg, Ca, P and K along with the essential elements (Mn, Fe, Cu and Zn) levelswas also reduced significantly. Reagent blanks from HF and TEA wereinsignificant (0.008 μg L−1) allowing a limit ofdetection of 0.004 μg L−1 or 0.26 ngg−1 Cd to be achieved (3σ, n = 6). Theperformance of the coprecipitation method (Scheme 3) was validated bydetermination of Cd in multivitamin/multielement tablets certified referencematerial (SRM 3280) by ID-ICP-MS. Experimental results (ngg−1) and recoveries were 78.8 ± 4.7(98.5%), 77.9 ± 5.2 (97.4%) and 76.5 ± 4.8(95.6%) for 110Cd, 111Cd and 114Cdisotopes, respectively. Several commercial MVM supplements were analyzed usingthe method. Mean Cd concentration ranged from 21.4 ng g−1 to93.3 ng g−1. These values are much lower than those reportedto date for various MVM supplements by ICP-MS determinations without chemicalseparation.
机译：在本文中，我们研究了基于Mg（OH）2和CaF2沉淀的三种不同的顺序共沉淀方案，分别使用三乙胺（TEA）和氢氟酸（HF）来测定多种维生素/矿物（MVM）中的镉（Cd）杂质通过同位素稀释（ID）电感耦合等离子体质谱（ICP-MS）进行补充。该方案涉及与TEA单独或与HF组合使用的三步共沉淀方案，根据方案分别命名为方案1（TEA-TEA-TEA），方案2（TEA-HF-TEA）和方案3（HF-TEA-TEA）每种试剂的添加顺序。用多元素标准溶液中掺有60μgL -1 Cd的MVM溶液进行了实验。所有方案都提供了从MVM基质中定量分离Cd的方法。方案1在去除干扰性伴随元素钼（Mo）和锡（Sn）方面效果最差。方案2对于Sn表现更好，但是在消除Mo方面失败。方案3在消除Mo和Sn中最有效。测试MVM溶液中的Mo含量从4.3μgmL -1 降低至0.014μgmL -1 ，而Sn的Mo含量则从0.5μgmL -1 至0.018μgmL −1 可以实现Cd的无干扰测定。盐矩阵到期到镁，钙，磷和钾以及必需元素（锰，铁，铜和锌）的含量也大大减少了。 HF和TEA的试剂空白为微不足道（0.008μgL −1 ）的限制为检测到0.004μgL -1 或0.26 ngg -1 Cd达到（3σ，n = 6）。的共沉淀法（方案3）的性能通过以下方法验证多种维生素/多种元素片剂中镉的测定参考ID-ICP-MS提供的材料（SRM 3280）。实验结果（ngg −1 ），回收率为78.8±4.7（98.5％），77.9±5.2（97.4％）和76.5±4.8（sup> 110 Cd， 111 Cd和 114 Cd的比例（95.6％）同位素。使用以下工具分析了几种商业MVM补充剂方法。平均Cd浓度范围为21.4 ng g -1 至93.3 ng g -1 。这些值远低于报告的值迄今为止，通过ICP-MS测定无需化学试剂即可获得各种MVM补充剂分离。

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