Digestion and extraction of biological materials for zinc stable isotope determination by inductively coupled plasma mass spectrometry
Digestion and extraction of biological materials for zinc stable isotope determination by inductively coupled plasma mass spectrometry
复制标题
DOI：
10.1039/ja9961100727
复制
发表时间：
1996-09-01
影响因子：
3.4
通讯作者：
MoserVeillon, PB
中科院分区：
文献类型：
--
作者：
Veillon, C;Patterson, KY;MoserVeillon, PB
描述了一种分离方法，用于快速去除锌从干扰基质成分，如氯化物，从消化的生物样品，然后通过ICP-MS测定锌的稳定同位素。该方法采用螯合的锌与三氟乙酰丙酮（TFA），萃取的螯合物与己烷，破坏的螯合物和溶解的锌到硝酸中进行测定。实现了锌与基质盐的完全分离，并且该方法不使用如在早期类似方案中所使用的氯化烃溶剂。由于Ce-140（2+）的存在，在测量Zn-70时，发现用于样品消解的硼硅酸盐玻璃管中的铈是一个潜在的问题。通过使用石英消解管和/或通过监测m/z 140校正任何铈，可以避免这种潜在的问题。通过一个独立的方法验证了准确性，并给出了使用锌的稳定同位素作为人体代谢的代谢示踪剂的例子。ID方法的检测限（空白3s）为0.7 μ g Zn。通过ID检测发现内部尿液池含有1.18 +/- 0.005 μ g g（-1）的锌（n = 3），通过AAS检测发现内部尿液池含有1.17 +/- 0.006 μ g g（-1）的锌（n = 3）。
A separation method is described for rapidly removing zinc from interfering matrix components, such as chloride, from digested biological samples prior to measurement of zinc stable isotopes by ICP-MS. The method employs chelation of the zinc with trifluoroacetylacetone (TFA), extraction of the chelate with hexane, destruction of the chelate and dissolution of the zinc into nitric acid for determination. Complete separation of the zinc from matrix salts is achieved, and the method does not employ chlorinated hydrocarbon solvents as used in earlier, similar schemes. Cerium from borosilicate glass tubes used in sample digestion was found to be a potential problem when measuring Zn-70, owing to the presence of Ce-140(2+). This potential problem can be avoided by using quartz digestion tubes and/or correcting for any cerium by monitoring m/z 140. Accuracy was verified by an independent method, and examples of the use of stable isotopes of zinc as metabolic tracers in human metabolism are given. The detection limit for the ID method (3s of blank) was 0.7 mu g Zn. An in-house urine pool was found to contain 1.18 +/- 0.005 mu g g(-1) of Zn (n = 3) by ID and 1.17 +/- 0.006 mu g g(-1) of Zn (n = 3) by AAS.