Novel sample preparation technique based on functional nanofiber mat for sensitive and precise determination of phenolic environmental estrogens in environmental water
Novel sample preparation technique based on functional nanofiber mat for sensitive and precise determination of phenolic environmental estrogens in environmental water
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DOI：
10.1039/c5ay00422e
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发表时间：
2015-06
影响因子：
3.1
通讯作者：
Xiaoqing Li;Feifei Qi;F. Zhou;Bi-Yi Yang;H. Gao;F. Rong;Qingyu Xu
中科院分区：
文献类型：
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作者：
Xiaoqing Li;Feifei Qi;F. Zhou;Bi-Yi Yang;H. Gao;F. Rong;Qingyu Xu
本研究描述了一种新的酚类环境雌激素（PEEs），包括双酚A（BPA），壬基酚（NP）和辛基酚（OP），在环境水样中的样品制备技术。采用静电纺丝技术制备了一种肼改性聚丙烯腈（HM-PAN）复合材料。建立了一种圆盘固相萃取（SPE）方法，该方法以功能化聚乙烯为吸附剂，在高效液相色谱-串联质谱（HPLC-MS/MS）联用前对PEEs进行萃取。对影响吸附剂萃取效率的关键因素进行了试验和优化。在优化的条件下，采用自制的圆盘固相萃取装置，样品前处理简单、快速，吸附剂床质量（4.0 mg）和洗脱剂体积（600 μL）显著减少。目标PEE的检测限在0.01-0.03 ng mL−1（S/N = 3）范围内。用4个真实的环境水样验证了该方法的适用性，加标回收率在84.6%~ 101.9%之间，相对标准偏差≤ 8.6%（n = 6）。与现有的测定方法进行了比较，结果表明，所提出的方法具有更好的回收率，灵敏度和重现性。结果表明，HM-PAN固相萃取技术是一种灵敏、准确分析环境水样中PEEs的可行方法。
The present study describes a novel sample preparation technique for phenolic environmental estrogens (PEEs), including bisphenol A (BPA), nonylphenol (NP) and octylphenol (OP), in environmental water samples. A hydrazine-modified polyacrylonitrile (HM-PAN) nanofiber mat, with subsequent amino group functionalization, was prepared using the electrospinning technique. A disk solid-phase extraction (SPE) was developed utilizing the functional nanofiber mat as a sorbent for extraction of PEEs prior to high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The critical factors affecting the extraction efficiency of the sorbent for the target analytes were tested and optimized. Under optimized conditions, a simple and fast sample preparation procedure was achieved using a home-made disk SPE device, with noticeably reduced sorbent bed mass (4.0 mg) and eluent volume (600 μL). The detection limits for the targeted PEEs were in the range of 0.01–0.03 ng mL−1 (S/N = 3). We validated the applicability of the proposed method using four real environmental water samples and satisfactory spiked recoveries were achieved in the range of 84.6–101.9% with low RSD ≤ 8.6% (n = 6). A comparison of the present method with the existing methods for the determination of PEEs was made and the results showed that the proposed method had better recoveries, sensitivity and reproducibility. The results demonstrated that the HM-PAN nanofiber mat-based SPE technique was a viable alternative for sensitive and precise analysis of PEEs in environmental water.