Faculty of Sciences, Chemistry and Biochemistry Department and Centre of Chemistry and Biochemistry, University of Lisbon, Campo Grande Ed. C8, 1749-016 Lisbon, Portugal.
Anal Bioanal Chem. 2010 Dec;398(7-8):3155-63. doi: 10.1007/s00216-010-4256-9. Epub 2010 Oct 9.
In this contribution, bar adsorptive micro-extraction using polystyrene-divinylbenzene sorbent phase and in situ derivatization with pentafluorophenyl hydrazine, followed by liquid desorption and high-performance liquid chromatography-diode array detection (BAμE(PS-DVB)(PFPH in situ)-LD/HPLC-DAD), was developed for the determination of six short-chain carbonyl compounds (formaldehyde, acetaldehyde, propanal, acetone, butanone, and 2-hexenal) in drinking water matrices. PFPH presented very good specificity as an in situ derivatization agent for short-chain ketones and aldehydes in aqueous media, allowing the formation of adducts with remarkable sensitivity, selectivity and the absence of photodegradation. Assays performed on 30-mL water samples spiked at the 25.0 μg L(-1) levels, under optimized experimental conditions, yielded recoveries ranging from 47.4 ± 3.8% to 85.2 ± 3.8%, in which the PS-DVB proved to be a convenient sorbent phase. The analytical performance showed good accuracy, suitable precision (RSD < 13.0%), detection limits in between 47 and 132 ng L(-1) and remarkable linear dynamic ranges (r(2) > 0.9907) from 1.0 to 80.0 μg L(-1). By using the standard addition methodology, the application of the present method to drinking water samples treated with different disinfectants, namely, chloride, ozone and both, allowed very good performances to monitor these priority compounds at the trace level. The proposed methodology proved to be a feasible alternative for polar compound analysis, showing to be easy to implement, reliable, sensitive and requiring a low sample volume to monitor short-chain aldehydes and ketones in drinking water matrices.
在这项工作中，我们开发了一种使用聚苯乙烯-二乙烯基苯吸附剂相和原位衍生试剂五氟苯肼的棒状吸附微萃取方法（BAμE(PS-DVB)(PFPH in situ)-LD/HPLC-DAD），用于测定饮用水基质中的六种短链羰基化合物（甲醛、乙醛、丙醛、丙酮、丁酮和 2-己烯醛）。PFPH 作为一种在水介质中用于短链酮和醛的原位衍生试剂，具有非常好的特异性，允许形成具有显著灵敏度、选择性和无光降解的加合物。在优化实验条件下，对 30-mL 水样进行测定，在 25.0 μg L(-1)水平下进行加标，回收率在 47.4 ± 3.8%至 85.2 ± 3.8%之间，其中 PS-DVB 被证明是一种方便的吸附剂相。分析性能表现出良好的准确性、适当的精密度（RSD < 13.0%）、检测限在 47 和 132 ng L(-1)之间，以及显著的线性动态范围（r(2) > 0.9907），范围从 1.0 到 80.0 μg L(-1)。通过使用标准添加方法，本方法在经不同消毒剂处理的饮用水样品中的应用，即氯、臭氧和两者，均能很好地监测这些优先化合物的痕量水平。所提出的方法被证明是一种可行的分析极性化合物的替代方法，具有易于实施、可靠、灵敏和需要低样品体积的特点，可用于监测饮用水基质中的短链醛和酮。
