Corazza Gabriela, Merib Josias, Magosso Hérica A, Bittencourt Otávio R, Carasek Eduardo
Departamento de Química, Universidade Federal de Santa Catarina, Florianópolis, 88040-900, SC, Brazil.
Departamento de Química, Universidade Federal de Santa Catarina, Florianópolis, 88040-900, SC, Brazil.
J Chromatogr A. 2017 Sep 1;1513:42-50. doi: 10.1016/j.chroma.2017.07.050. Epub 2017 Jul 14.
In this study, the hybrid material 3-n-propyl(3-methylpyridinium) silsesquioxane chloride (Si3PyCl) was synthesized and investigated as a novel sorbent phase for the disposable pipette extraction (DPX) technique coupled to high-performance liquid chromatography-florescence detection. This sorbent phase was characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). Aqueous samples containing the phenolic endocrine-disrupting compounds bisphenol A (BPA), 17α-ethynylestradiol (EE2), 4-tert-octylphenol (4-t-OP), 4-octylphenol (4-OP) and 4-nonylphenol (4-NP) were subjected to DPX procedures and a series of optimizations was performed to determine the ideal extraction conditions using this approach. The proposed sorbent phase exhibited higher extraction efficiency than DPX-RP (reversed phase tips containing styrene-divinylbenzene), commonly used for the determination of the phenolic endocrine- disrupting-compounds under study. Satisfactory analytical performance was achieved with linear ranges from 2 to 100μgL for 4-t-OP and 1-100μgL for the other analytes. Limits of detection of 0.60μgL for 4-t-OP and 0.30μgL for other analytes, RSDs ranging from 1 to 20% and relative recoveries of 83-116% were obtained. Based on these satisfactory results, this sorbent phase represents a valuable alternative for the extraction of compounds with polar moieties in their structure.
在本研究中，合成了杂化材料3-正丙基（3-甲基吡啶鎓）倍半硅氧烷氯化物（Si3PyCl），并将其作为一种新型吸附剂相，用于与高效液相色谱-荧光检测联用的一次性移液器萃取（DPX）技术。通过扫描电子显微镜（SEM）和傅里叶变换红外光谱（FTIR）对该吸附剂相进行了表征。对含有酚类内分泌干扰化合物双酚A（BPA）、17α-乙炔雌二醇（EE2）、4-叔辛基苯酚（4-t-OP）、4-辛基苯酚（4-OP）和4-壬基苯酚（4-NP）的水样进行了DPX操作，并进行了一系列优化，以确定使用该方法的理想萃取条件。所提出的吸附剂相比常用于测定所研究的酚类内分泌干扰化合物的DPX-RP（含苯乙烯-二乙烯基苯的反相吸头）表现出更高的萃取效率。4-t-OP的线性范围为2至100μg/L，其他分析物的线性范围为1至100μg/L，获得了令人满意的分析性能。4-t-OP的检测限为0.60μg/L，其他分析物的检测限为0.30μg/L，相对标准偏差（RSD）范围为1%至20%，相对回收率为83%至116%。基于这些令人满意的结果，这种吸附剂相是萃取结构中带有极性部分的化合物的一种有价值的替代方法。
