Dugheri Stefano, Cappelli Giovanni, Fanfani Niccolò, Ceccarelli Jacopo, Marrubini Giorgio, Squillaci Donato, Traversini Veronica, Gori Riccardo, Mucci Nicola, Arcangeli Giulio
Industrial Hygiene and Toxicology Laboratory, University Hospital Careggi, 50134 Florence, Italy.
Department of Experimental and Clinical Medicine, University of Florence, 50121 Florence, Italy.
Molecules. 2023 Jul 16;28(14):5441. doi: 10.3390/molecules28145441.
Formaldehyde (FA) is a toxic compound and a human carcinogen. Regulating FA-releasing substances in commercial goods is a growing and interesting topic: worldwide production sectors, like food industries, textiles, wood manufacture, and cosmetics, are involved. Thus, there is a need for sensitive, economical, and specific FA monitoring tools. Solid-phase microextraction (SPME), with -(2,3,4,5,6-pentafluorobenzyl)-hydroxylamine (PFBHA) on-sample derivatization and gas chromatography, is proposed for FA monitoring of real-life samples. This study reports the use of polydimethylsiloxane (PDMS) as a sorbent phase combined with innovative commercial methods, such as multiple SPME (MSPME) and cooling-assisted SPME, for FA determination. Critical steps, such as extraction and sampling, were evaluated in method development. The derivatization was performed at 60 °C for 30 min, followed by 15 min sampling at 10 °C, in three cycles (SPME Arrow) or six cycles (SPME). The sensitivity was satisfactory for the method's purposes (LOD-LOQ at 11-36 ng L, and 8-26 ng L, for SPME and SPME Arrow, respectively). The method's linearity ranges from the lower LOQ at trace level (ng L) to the upper LOQ at 40 mg L. The precision range was 5.7-10.2% and 4.8-9.6% and the accuracy was 97.4% and 96.3% for SPME and SPME Arrow, respectively. The cooling MSPME set-up applied to real commercial goods provided results of quality comparable to previously published data.
甲醛（FA）是一种有毒化合物，也是一种人类致癌物。规范商业产品中甲醛释放物质是一个日益受到关注且有趣的话题：全球各生产领域，如食品工业、纺织业、木材制造业和化妆品行业都涉及其中。因此，需要灵敏、经济且特异的甲醛监测工具。本文提出采用在样品上进行衍生化的 -(2,3,4,5,6 - 五氟苄基)-羟胺（PFBHA）与气相色谱联用的固相微萃取（SPME）技术，用于实际样品中甲醛的监测。本研究报告了使用聚二甲基硅氧烷（PDMS）作为吸附相，并结合多种创新商业方法，如多次固相微萃取（MSPME）和冷却辅助固相微萃取，来测定甲醛。在方法开发过程中，对萃取和采样等关键步骤进行了评估。衍生化在60°C下进行30分钟，随后在10°C下进行15分钟采样，分三个循环（SPME Arrow）或六个循环（SPME）进行。该方法的灵敏度对于其目的而言是令人满意的（SPME和SPME Arrow的检测限 - 定量限分别为11 - 36 ng/L和8 - 26 ng/L）。该方法的线性范围从痕量水平（ng/L）的较低定量限到40 mg/L的较高定量限。SPME和SPME Arrow的精密度范围分别为5.7 - 10.2%和4.8 - 9.6%，准确度分别为97.4%和96.3%。应用于实际商业产品的冷却MSPME装置所提供的结果质量与先前发表的数据相当。
