Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran.
School of Chemistry, College of Science, University of Tehran, P.O. Box 14155-6455, Tehran, Iran.
Anal Bioanal Chem. 2022 Mar;414(6):2285-2296. doi: 10.1007/s00216-021-03868-6. Epub 2022 Jan 5.
The current study presents a periodic mesoporous organosilica (PMO) with a high surface area and uniform-porosity material. The PMO materials were successfully synthesized and modified. The resultant material was characterized by different characterization techniques. The prepared PMO was immobilized on a stainless steel wire surface and was evaluated for headspace solid-phase microextraction of the ultra-trace amount of phthalate esters from saliva and polyethylene terephthalate containers which were in contact with hot and cold water. Separation and determination of the phthalate esters (PEs) were performed by the GC-FID and GC-MS instruments. The key parameters affecting the extraction efficiencies, including extraction temperature, extraction time, ionic strength, and desorption temperature and time, were investigated and optimized. Under optimum conditions, the repeatability for one fiber (n = 7) was 4.8-8.7%, and fiber-to-fiber reproducibility (n = 3) was 7.5-10.6% for the extracted compounds. The limits of detection of the developed method for the studied compounds were between 0.01 and 1 μg L. The results showed suitable coefficients of determination (R ≥ 0.99) for all of the analytes in the 0.05-300 μg L calibration range. Acceptable recovery values of 91-107%, 82-110%, and 98-104% were obtained in saliva, polyethylene terephthalate containers hot water, and cold water, respectively.
本研究提出了一种具有高表面积和均匀孔结构的周期性介孔有机硅(PMO)材料。成功合成并修饰了 PMO 材料。采用不同的表征技术对所得材料进行了表征。将制备的 PMO 固定在不锈钢丝表面上,并用于顶空固相微萃取法从唾液和与热水和冷水接触的聚对苯二甲酸乙二醇酯容器中痕量邻苯二甲酸酯的萃取。通过 GC-FID 和 GC-MS 仪器对邻苯二甲酸酯(PE)进行了分离和测定。研究并优化了影响萃取效率的关键参数,包括萃取温度、萃取时间、离子强度以及解吸温度和时间。在最佳条件下,对于提取的化合物,一根纤维(n=7)的重复性为 4.8-8.7%,纤维间重现性(n=3)为 7.5-10.6%。该方法对研究化合物的检出限在 0.01-1μg L 之间。结果表明,在所研究的 0.05-300μg L 校准范围内,所有分析物的相关系数(R≥0.99)均合适。在唾液、聚对苯二甲酸乙二醇酯容器热水和冷水中,回收率分别为 91-107%、82-110%和 98-104%。