Ishak Ismarulyusda, Rosli Farah Dayana, Mohamed Jamaludin, Mohd Ismail Muhammad Faiz
Biomedical Science Programme, Faculty of Health Sciences, School of Diagnostic and Applied Health Sciences, Universiti Kebangsaan Malaysia, Jalan Raja Muda Abdul Aziz, 50300 Kuala Lumpur, Malaysia.
Malays J Med Sci. 2015 Nov;22(6):11-20.
Microwave is the most reliable sample digestion method. However, it requires expensive microwave digester automation and has relatively low productivity. In this study, three non-automated digestion methods, i.e. wet acid digestion using nitric acid (HNO) and hydrogen peroxide (HO), wet acid digestion using HNO, and dry washing, are compared in order to determine the best approach.
Certified reference material IAEA-086 (International Atomic Energy Agency, Austria) and hair and nail samples from 20 female students of Universiti Kebangsaan Malaysia, aged 19 to 30 years, were collected and analysed using the three digestion methods.
For hair samples, analysis of variance of repeated measures showed significant differences in the level of all elements ( < 0.001) between the three methods. For nail samples, only the copper (Cu) level showed no significant difference ( = 0.100) between methods. Wet acid digestion using HNO and HO showed the best within- and between-run relative standard deviation (RSD) values, with within-run RSD for all elements, except for selenium (Se), < 5%. The between-run precision ranges from 6.14% to 17.96% for hair and from 3.53% to 11.52% for nail samples. Wet acid digestion using HNO and HO showed both good accuracy and precision for manganese (Mn) and magnesium (Mg), with percentage recoveries of 110% and 96.9%, respectively. All elements show higher method detection limit (MDL) values than the previous study: 0.05 μg/g Mg for wet acid digestion using HNO, 0.02 μg/g Se for wet acid digestion using HNO and HO, and 0.2 μg/g Mg for dry ash method.
Wet acid digestion using HNO and HO proved to be the best method in terms of precision, accuracy, recovery, and MDL. However, only Mn and Mg showed adequate precision, accuracy, and percentage of recovery.
微波是最可靠的样品消解方法。然而,它需要昂贵的微波消解仪自动化设备,且生产率相对较低。在本研究中,比较了三种非自动化消解方法,即使用硝酸(HNO₃)和过氧化氢(H₂O₂)的湿酸消解、使用HNO₃的湿酸消解以及干灰化法,以确定最佳方法。
收集了国际原子能机构(奥地利)的认证参考物质IAEA - 086以及马来西亚国民大学20名年龄在19至30岁之间的女学生的头发和指甲样本,并使用这三种消解方法进行分析。
对于头发样本,重复测量的方差分析表明,三种方法之间所有元素的含量存在显著差异(P < 0.001)。对于指甲样本,只有铜(Cu)含量在各方法之间没有显著差异(P = 0.100)。使用HNO₃和H₂O₂的湿酸消解显示出最佳的批内和批间相对标准偏差(RSD)值,除硒(Se)外,所有元素的批内RSD < 5%。头发的批间精密度范围为6.14%至17.96%,指甲样本的批间精密度范围为3.53%至11.52%。使用HNO₃和H₂O₂的湿酸消解对锰(Mn)和镁(Mg)显示出良好的准确度和精密度,回收率分别为110%和96.9%。所有元素的方法检出限(MDL)值均高于先前的研究:使用HNO₃的湿酸消解中镁(Mg)的MDL为0.05 μg/g,使用HNO₃和H₂O₂的湿酸消解中硒(Se)的MDL为0.02 μg/g,干灰化法中镁(Mg)的MDL为0.2 μg/g。
就精密度、准确度、回收率和MDL而言,使用HNO₃和H₂O₂的湿酸消解被证明是最佳方法。然而,只有Mn和Mg显示出足够的精密度、准确度和回收率百分比。