Wang Tiebang, Jia Xiujuan, Wu Jane
Analytical Research Department, Merck Research Laboratories, P.O. Box 2000, R80L-115, Rahway, NJ 07065-0900, USA.
J Pharm Biomed Anal. 2003 Nov 24;33(4):639-46. doi: 10.1016/s0731-7085(03)00357-1.
A simple method for the simultaneous determination of up to 21 elements in organic matrices is proposed. Organic samples are simply dispersed in concentrated nitric acid by sonication, and the resulting emulsions/suspensions are directly aspirated into an inductively coupled plasma atomic emission spectrometer (ICP-AES) calibrated with aqueous standards for analysis. Proof of concept was provided by the excellent recoveries for the analysis of a 21-element metallo-organic standard. In addition, the results obtained using this method for a waste oil sample compared favorably with those from a method that utilized microwave digestion for sample preparation. Comparable results were also obtained by dilution in an organic solvent followed by ICP-AES analysis with an ultrasonic nebulizer equipped with a membrane desolvator. Furthermore, the viability and validity of this method were confirmed by the analysis of the National Institute of Standards and Technology standard reference material 1084a Wear-Metals in Lubricating Oil. Spike recoveries ranged from 83 to 105% and the limits of quantitation were 6 microg g(-1) or less for all the elements analyzed.
提出了一种同时测定有机基质中多达21种元素的简单方法。通过超声处理将有机样品简单地分散在浓硝酸中,然后将所得乳液/悬浮液直接吸入用含水标准溶液校准的电感耦合等离子体原子发射光谱仪(ICP-AES)中进行分析。对一种21元素金属有机标准品的分析具有出色的回收率,从而提供了概念验证。此外,使用该方法对废油样品进行分析得到的结果与采用微波消解进行样品制备的方法所得结果相比具有优势。通过在有机溶剂中稀释,然后使用配备膜去溶剂器的超声雾化器进行ICP-AES分析,也获得了可比的结果。此外,通过对美国国家标准与技术研究院标准参考物质1084a润滑油中的磨损金属进行分析,证实了该方法的可行性和有效性。加标回收率在83%至105%之间,所有分析元素的定量限均为6μg g⁻¹或更低。