Ansari Dogaheh Mehdi, Behzadi Mansoureh
Department of Pharmaceutics, Faculty of Pharmacy, Kerman Medical Science University, Kerman, Iran.
Department of Chemistry, Faculty of Science, Shahid Bahonar University of Kerman, Kerman, Iran.
J Pharm Anal. 2019 Jun;9(3):185-192. doi: 10.1016/j.jpha.2019.03.006. Epub 2019 Mar 15.
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.
本文描述了用于双酚A和五种邻苯二甲酸酯直接固相微萃取的聚磷酸盐掺杂聚吡咯/纳米二氧化硅纳米复合涂层在钢丝上的电沉积。我们优化了影响纳米复合材料萃取效率和形貌的参数,如沉积电位、吡咯和聚磷酸盐的浓度、沉积时间以及纳米二氧化硅的用量。在优化条件下,通过扫描电子显微镜和傅里叶变换红外光谱对纳米复合材料进行了表征。此外,还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值。随后,通过热解吸气相色谱 - 质谱联用对所提出的方法进行了验证,并获得了可接受的品质因数。校准曲线的线性范围为0.01至50 ng/mL,相关系数可接受(0.9956 - 0.9987),检测限在0.002至0.01 ng/mL范围内。对于含有0.1 ng/mL目标分析物的水溶液,通过五次重复分析得到的日内和日间相对标准偏差分别在3.3% - 5.4%和5% - 7.1%范围内。对在相同条件下制备的三种不同纤维测量了纤维间的重现性,结果在7.3%至9.8%之间。此外,两种不同浓度下的萃取回收率≥96%。最后,通过将所提出的方法应用于一些眼药水和注射液的分析,证明了该方法的适用性。