分析序列中的样品制备会增加错误的数量,非常耗时,涉及危险试剂的操纵。因此,当需要改进分析方法时,样品制备步骤需要优化或重新设计。此外,此步骤可能涉及大量有毒试剂和大量废物。在这方面,这项研究提出了一种基于微波辅助湿法消解的新方法,该方法结合了两种绿色策略:小型化系统(体积为几微升)和仅使用过氧化氢。三个生物样本(人血清,尿液,和植物体外材料)是由于它们对疾病监测的高潜力而选择的,毒理学研究,和生物技术应用。几种微量元素(Ca,Cd,Co,Cu,Fe,Mg,Mn,Mo,Ni,Se,和Zn)通过电感耦合等离子体发射光谱和电感耦合等离子体质谱法测定。对于人体血清和尿液,使用经过认证的参考材料来检查准确性;回收率从72%(Cd,ICP-MS)至105%(Mg,ICPOES)用于血清,而尿液,它们从82%(Ni,ICP-MS)至122%(Zn,ICP-MS)。对于大豆愈伤组织样品(离体植物材料),对所提出的方法和酸消化方法进行了比较,以评估准确性,结果一致。检出限为0.001-60µgL-1(Cd最低),从而证明了合适的灵敏度。此外,分解效率是通过测定残余碳来证明的,并且在消化的最终产物中发现低量(低于0.8%wv-1)。对所提出的方法进行了绿色度量方法的计算,根据AGREEPrep软件,发现大约是0.4。最后,该方法适用于收集的COVID-19患者的尿液样本和用银纳米颗粒培养的大豆愈伤组织。这种样品制备方法是涉及生物样品的元素分析的一种新的无酸和小型化替代方法。
Sample preparation in an analytical sequence increases the number of errors, is highly time-consuming, and involves the manipulation of hazardous reagents. Therefore, when an improvement in an analytical method is required, the sample preparation step needs to be optimised or redesigned. Moreover, this step can involve significant toxic reagents and a high volume of waste. In that regard, this study proposes a new procedure based on microwave-assisted wet digestion combining two green strategies: a miniaturised system (with a few microlitres of volume) and the only use of hydrogen peroxide. Three biological samples (human serum, urine, and plant in vitro material) were chosen due to their high potential for disease monitoring, toxicological studies, and biotechnology applications. Several trace elements (Ca, Cd, Co, Cu, Fe, Mg, Mn, Mo, Ni, Se, and Zn) were determined by inductively coupled plasma optical emission spectroscopy and inductively coupled plasma mass spectrometry. For human serum and urine, a certified reference material was used to check for accuracy; the recovery ranged from 72% (Cd, ICP-MS) to 105% (Mg, ICP OES) for serum, while for urine, they varied from 82% (Ni, ICP-MS) to 122% (Zn, ICP-MS). For the soybean callus sample (in vitro plant material), a comparison between the proposed method and the acid digestion method was conducted to evaluate the accuracy, and the results agreed. The detection limits were 0.001-60 µg L-1 (lowest for Cd), thus demonstrating a suitable sensitivity. Moreover, the decomposition efficiency was demonstrated by determining the residual carbon, and a low amount was found in the final product digested (below 0.8% w v-1). A green metric approach was calculated for the proposed method, and according to AGREEprep software, it was found to be around 0.4. Finally, the method was applied to urine samples collected in patients with COVID-19 and soybean callus cultivated with silver nanoparticles. This sample preparation method is a new acidless and miniaturised alternative for elemental analysis involving biological samples.