Brandão Pedro F, Ramos Rui M, Valente Inês M, Almeida Paulo J, Carro Antonia M, Lorenzo Rosa A, Rodrigues José A
REQUIMTE/LAQV - Departamento de Química e Bioquímica, Faculdade de Ciências da Universidade do Porto, Rua do Campo Alegre, 687, 4169-007, Porto, Portugal.
REQUIMTE/LAQV-ICBAS - Departamento de Clínicas Veterinárias, Instituto de Ciências Biomédicas Abel Salazar, Universidade do Porto, R. Jorge de Viterbo Ferreira 228, 4050-343, Porto, Portugal.
Anal Bioanal Chem. 2017 Apr;409(11):2885-2892. doi: 10.1007/s00216-017-0233-x. Epub 2017 Feb 11.
In this work, a simple methodology was developed for the extraction and determination of free formaldehyde content in cork agglomerate samples. For the first time, gas-diffusion microextraction was used for the extraction of volatile formaldehyde directly from samples, with simultaneous derivatization with acetylacetone (Hantzsch reaction). The absorbance of the coloured solution was read in a spectrophotometer at 412 nm. Different extraction parameters were studied and optimized (extraction temperature, sample mass, volume of acceptor solution, extraction time and concentration of derivatization reagent) by means of an asymmetric screening. The developed methodology proved to be a reliable tool for the determination of formaldehyde in cork agglomerates with the following suitable method features: low LOD (0.14 mg kg) and LOQ (0.47 mg kg), r = 0.9994, and intraday and interday precision of 3.5 and 4.9%, respectively. The developed methodology was applied to the determination of formaldehyde in different cork agglomerate samples, and contents between 1.9 and 9.4 mg kg were found. Furthermore, formaldehyde was also determined by the standard method EN 717-3 for comparison purposes; no significant differences between the results of both methods were observed. Graphical abstract Representation of the GDME system and its main components.
在本研究中,开发了一种简单的方法用于提取和测定软木聚集体样品中的游离甲醛含量。首次采用气体扩散微萃取法直接从样品中提取挥发性甲醛,并同时与乙酰丙酮进行衍生化反应(汉茨希反应)。在分光光度计上于412nm处读取有色溶液的吸光度。通过非对称筛选研究并优化了不同的萃取参数(萃取温度、样品质量、接受液体积、萃取时间和衍生化试剂浓度)。所开发的方法被证明是一种可靠的工具,用于测定软木聚集体中的甲醛,具有以下合适的方法特性:低检测限(0.14mg/kg)和定量限(0.47mg/kg),r = 0.9994,日内和日间精密度分别为3.5%和4.9%。所开发的方法应用于测定不同软木聚集体样品中的甲醛,发现含量在1.9至9.4mg/kg之间。此外,为了进行比较,还采用标准方法EN 717-3测定甲醛;两种方法的结果之间未观察到显著差异。图形摘要气体扩散微萃取系统及其主要组件的示意图。