This paper describes the electrodeposition of polyphosphate-doped polypyrrole/nanosilica nanocomposite coating on steel wire for direct solid-phase microextraction of bisphenol A and five phthalates. We optimized influencing parameters on the extraction efficiency and morphology of the nanocomposite such as deposition potential, concentration of pyrrole and polyphosphate, deposition time and the nanosilica amount. Under the optimized conditions, characterization of the nanocomposite was investigated by scanning electron microscopy and Fourier transform infra-red spectroscopy. Also, the factors related to the solid-phase microextraction method including desorption temperature and time, extraction temperature and time, ionic strength and pH were studied in detail. Subsequently, the proposed method was validated by gas chromatography-mass spectrometry by thermal desorption and acceptable figures of merit were obtained. The linearity of the calibration curves was between 0.01 and 50 ng/mL with acceptable correlation coefficients (0.9956–0.9987) and limits of detection were in the range 0.002–0.01 ng/mL. Relative standard deviations in terms of intra-day and inter-day by five replicate analyses from aqueous solutions containing 0.1 ng/mL of target analytes were in the range 3.3%–5.4% and 5%–7.1%, respectively. Fiber-to-fiber reproducibilities were measured for three different fibers prepared in the same conditions and the results were between 7.3% and 9.8%. Also, extraction recoveries at two different concentrations were ≥96%. Finally, the suitability of the proposed method was demonstrated through its application to the analysis of some eye drops and injection solutions.

本文介绍了在钢丝上电沉积多磷酸盐掺杂的聚吡咯/纳米二氧化硅纳米复合涂层，用于直接固相微萃取双酚 A 和五种邻苯二甲酸酯。我们优化了影响纳米复合材料提取效率和形态的参数，如沉积电位、吡咯和聚磷酸盐的浓度、沉积时间和纳米二氧化硅的量。在优化的条件下，通过扫描电子显微镜和傅里叶变换红外光谱研究了纳米复合材料的表征。并详细研究了与固相微萃取方法相关的因素，包括解吸温度和时间、萃取温度和时间、离子强度和pH。随后，所提出的方法通过热解吸的气相色谱-质谱法进行了验证，并获得了可接受的品质因数。校准曲线的线性在 0.01 和 50 ng/mL 之间，相关系数可接受 (0.9956–0.9987)，检测限在 0.002–0.01 ng/mL 范围内。对含有 0.1 ng/mL 目标分析物的水溶液进行五次重复分析，在日内和日间的相对标准偏差分别在 3.3%–5.4% 和 5%–7.1% 范围内。测量在相同条件下制备的三种不同纤维的纤维间重现性，结果在 7.3% 和 9.8% 之间。此外，两种不同浓度的萃取回收率均≥96%。最后，