Facultad de Ciencias Exactas, UNLP, CONICET, Laboratorio de Investigación y Desarrollo de Métodos Analíticos (LIDMA) y División Química Analítica, Calle 47 esq. 115, La Plata B1900AJL, Argentina.
Facultad de Ciencias Exactas, UNLP, CONICET, Laboratorio de Investigación y Desarrollo de Métodos Analíticos (LIDMA) y División Química Analítica, Calle 47 esq. 115, La Plata B1900AJL, Argentina.
J Chromatogr A. 2022 Aug 30;1679:463397. doi: 10.1016/j.chroma.2022.463397. Epub 2022 Aug 8.
A simple, sensitive and reproducible solid-phase extraction method using plastic cartridges containing a monolithic sorbent (m-SPE), coupled to reverse phase liquid chromatography analysis, aiming to determine fifteen polycyclic aromatic hydrocarbons in surface water samples, was developed. The sorbent was easily prepared through a thermal polymerization reaction by using a mixture of n-butyl methacrylate as non-polar monomer and ethylene glycol dimethacrylate as crosslinker contained in a typical Polypropylene syringe cartridge. The effect of different parameters (type of hydrophobic monomer, elution solvent, sample volume, sorbent amount and sorbent load capacity) on the extraction efficiency was optimized. The optimal conditions were achieved by using n-butyl methacrylate as monomer, tetrahydrofurane (THF) as solvent for sorbent cleaning, THF:acetone (1:1) as elution solvent, 25.00 mL of sample volume, 600 µL of the polymerization mixture and 60 µg L as sample loading capacity. Finally, the sorbent charge capacity, the reusability of the cartridges and the extraction efficiency of the m-SPE monolith, as compared with a typical C8 cartridge, were evaluated. Under the optimized experimental conditions, enrichment factors were between 76 and 103, relative recovery factors from 78 to 103%, accuracy values in the range of 58 to 98%, and inter-batch reproducibility values from between 2 and 10%, were obtained. The limits of detection and quantification were obtained by two different procedures: the signal to noise (S/N) ratios (3 and 10, respectively) and the IUPAC convention. The lowest LOD and LOQ values, obtained with the S/N ratios, were between 0.02 and 1.00 µg L, respectively whereas with the IUPAC convention the values were between 0.07 and 5 µg L. Using this procedure, several PAHs could be detected in the surface water sample taken from a river stream located in La Plata city (Buenos Aires Province, Argentina).
开发了一种简单、灵敏且重现性好的固相萃取方法，使用含有整体式吸附剂 (m-SPE) 的塑料小柱，与反相液相色谱分析相结合，旨在测定地表水样品中的十五种多环芳烃。吸附剂通过热聚合反应轻松制备，使用混合的正丁基甲基丙烯酸酯作为非极性单体和乙二醇二甲基丙烯酸酯作为交联剂，包含在典型的聚丙烯注射器小柱中。优化了不同参数（疏水性单体类型、洗脱溶剂、样品体积、吸附剂用量和吸附剂负载容量）对萃取效率的影响。通过使用正丁基甲基丙烯酸酯作为单体、四氢呋喃 (THF) 作为吸附剂清洗溶剂、THF:丙酮 (1:1) 作为洗脱溶剂、25.00 mL 样品体积、600 µL 聚合混合物和 60 µg L 作为样品加载容量，达到了最佳条件。最后，评估了吸附剂的电荷容量、小柱的可重复使用性以及 m-SPE 整体式的萃取效率，与典型的 C8 小柱相比。在优化的实验条件下，富集因子在 76 到 103 之间，相对回收率因子在 78 到 103%之间，准确度值在 58 到 98%之间，批间重现性值在 2 到 10%之间。通过两种不同的程序获得了检测限和定量限：信噪比（分别为 3 和 10）和 IUPAC 公约。使用信噪比获得的最低检测限和定量限分别在 0.02 和 1.00 µg L 之间，而使用 IUPAC 公约获得的最低检测限和定量限分别在 0.07 和 5 µg L 之间。使用该程序，可以在取自阿根廷拉普拉塔市（布宜诺斯艾利斯省）一条河流的地表水样品中检测到几种多环芳烃。
