Salvador A, Pascual-Martí M C, Aragó E, Chisvert A, March J G
Departamento de Quimica Analitica, Facultad de Quimica, Universitat de València, 46100 Burjassot, Valencia, Spain.
Talanta. 2000 May 5;51(6):1171-7. doi: 10.1016/s0039-9140(00)00290-3.
Microwave assisted pre-treatments for atomic spectrometric determination (inductive coupled plasma-optical emission spectrometry, ICP-OES or flame atomic absorption spectrometry, FAAS) of metallic elements, usually present in antidandruff shampoos, are proposed. They are based on the digestion of the sample with HNO(3) into a closed reactor, which is irradiated at 800 W for a few minutes. Selenium was determined by ICP-OES. The limit of detection was 0.11 mg l(-1); the relative standard deviation (R.S.D.) for the selenium content in the samples was in the 0.6-3.6% range. The results obtained were in agreement with the label contents and the recovery of the proposed method was in the 100-106% range. Zinc and cadmium were determined by FAAS. The limit of detection for zinc determination was 0.078 mg l(-1); the R.S.D. for zinc contents was in the 0.8-8.6% range. A limit of detection of 0.09 mg l(-1) was obtained for cadmium determination; the R.S.D. for cadmium contents was in the 0.7-2.7% range. The determinations were performed after two different sample mineralization pre-treatments - dry ashing (in an electric furnace) and wet mineralization (in a microwave oven). Both methodologies provided comparable results for zinc and cadmium determination in shampoos. The proposed microwave assisted digestion procedures allow a precise and accurate determination of selenium, zinc and cadmium in commercial antidandruff shampoos, and the sample pre-treatment is less time-consuming than the classic methods.
本文提出了用于测定去屑洗发水中常见金属元素(采用电感耦合等离子体发射光谱法(ICP - OES)或火焰原子吸收光谱法(FAAS)进行原子光谱测定)的微波辅助预处理方法。这些方法基于在封闭反应器中用硝酸(HNO₃)对样品进行消解,然后在800W功率下辐照几分钟。采用ICP - OES测定硒。检测限为0.11mg l⁻¹;样品中硒含量的相对标准偏差(R.S.D.)在0.6 - 3.6%范围内。所得结果与标签标注含量一致,该方法的回收率在100 - 106%范围内。采用FAAS测定锌和镉。锌测定的检测限为0.078mg l⁻¹;锌含量的R.S.D.在0.8 - 8.6%范围内。镉测定的检测限为0.09mg l⁻¹;镉含量的R.S.D.在0.7 - 2.7%范围内。测定是在两种不同的样品矿化预处理后进行的——干灰化(在电炉中)和湿矿化(在微波炉中)。两种方法在测定洗发水中的锌和镉时提供了可比的结果。所提出的微波辅助消解程序能够精确、准确地测定市售去屑洗发水中的硒、锌和镉,并且样品预处理比传统方法耗时更少。