Mirzajani Roya, Kardani Fatemeh
Chemistry Department, College of Science, Shahid Chamran University, Ahvaz, Iran.
Chemistry Department, College of Science, Shahid Chamran University, Ahvaz, Iran.
J Pharm Biomed Anal. 2016 Apr 15;122:98-109. doi: 10.1016/j.jpba.2016.01.046. Epub 2016 Jan 23.
A molecularly imprinted polymer (MIP) fiber on stainless steel wire using ciprofloxacin template with a mild template removal condition was synthetized and evaluated for fiber solid phase microextraction (SPME) of fluoroquinolones (FQs) from biological fluids and pharmaceutical samples, followed by high performance liquid chromatography analysis with UV detection (HPLC-UV). The developed MIP fiber exhibited high selectivity for the analytes in complex matrices. The coating of the fibers were inspected using fourier transform infrared spectrophotometry, thermogaravimetric analysis, energy dispersive X-ray (EDX) spectroscopy as well as by scanning electron microscopy (SEM). The fiber shows high thermal stability (up to 300°C), good reproducibility and long lifetime. The composite coating did not swell in organic solvents nor did it strip off from the substrate. It was also highly stable and extremely adherent to the surface of the stainless steel fiber. The fabricated fiber exclusively exhibited excellent extraction efficiency and selectivity for some FQs. The effective parameters influencing the microextraction efficiency such as pH, extraction time, desorption condition, and stirring rate were investigated. Under optimized conditions, the limits of detection of the four FQs ranged from 0.023-0.033 μg L(-1) (S/N=5) and the calibration graphs were linear in the concentration range from 0.1-40 μg L(-1), the inter-day and intraday relative standard deviations (RSD) for various FQs at three different concentration level (n=5) using a single fiber were 1.1-4.4% and the fiber to fiber RSD% (n=5) was 4.3-6.7% at 5 μg L(-1) of each anlyetes. The method was successfully applied for quantification of FQs in real samples including serum, plasma and tablet formulation with the recoveries between 97 to 102%.
以环丙沙星为模板，在温和的模板去除条件下，合成了一种基于不锈钢丝的分子印迹聚合物（MIP）纤维，并将其用于生物流体和药物样品中氟喹诺酮类药物（FQs）的纤维固相微萃取（SPME），随后采用高效液相色谱 - 紫外检测法（HPLC - UV）进行分析。所制备的MIP纤维对复杂基质中的分析物表现出高选择性。采用傅里叶变换红外光谱法、热重分析、能量色散X射线（EDX）光谱以及扫描电子显微镜（SEM）对纤维涂层进行了检测。该纤维具有高热稳定性（高达300°C）、良好的重现性和较长的使用寿命。复合涂层在有机溶剂中不溶胀，也不会从基底上脱落。它还具有高度稳定性，并且与不锈钢纤维表面紧密结合。所制备的纤维对某些氟喹诺酮类药物表现出优异的萃取效率和选择性。研究了影响微萃取效率的有效参数，如pH值、萃取时间、解吸条件和搅拌速率。在优化条件下，四种氟喹诺酮类药物的检测限为0.023 - 0.033 μg L⁻¹（S/N = 5），校准曲线在0.1 - 40 μg L⁻¹浓度范围内呈线性，使用单根纤维在三个不同浓度水平（n = 5）下对各种氟喹诺酮类药物进行日间和日内相对标准偏差（RSD）为1.1 - 4.4%，在每种分析物浓度为5 μg L⁻¹时，纤维间RSD%（n = 5）为4.3 - 6.7%。该方法成功应用于血清、血浆和片剂等实际样品中氟喹诺酮类药物的定量分析，回收率在97%至102%之间。
