Asgharinezhad Ali Akbar, Mollazadeh Narges, Ebrahimzadeh Homeira, Mirbabaei Fatemeh, Shekari Nafiseh
Faculty of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran, Iran.
Faculty of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran, Iran.
J Chromatogr A. 2014 Apr 18;1338:1-8. doi: 10.1016/j.chroma.2014.02.027. Epub 2014 Feb 18.
The coextraction of acidic and basic drugs from different samples is a considerable and disputable concept in sample preparation strategies. In this study, for the first time, simultaneous extraction of acidic and basic drugs with magnetic nanoparticles based dispersive micro-solid phase extraction followed by high performance liquid chromatography-ultraviolet detection was introduced. Cetyltrimethyl ammonium bromide-coated Fe3O4@decanoic acid as an efficient sorbent was successfully applied to adsorb diclofenac (DIC) as an acidic and diphenhydramine (DPH) as a basic model compound. First, appropriate amount of synthetic Fe3O4@decanoic acid nanoparticles was added to aqueous solution of drugs. After adjusting the pH of the solution, cetyltrimethyl ammonium bromide (CTAB) was added to the mixture being stirred at a constant rate. After the adsorption of drugs and decantation of supernatant with a magnetic field, the sorbent was eluted with methanol by fierce vortex. The parameters affecting the extraction efficiency were optimized and obtained as: pH of the sample=9, concentration of CTAB=0.2mmolL(-1), amount of sorbent=10mg, extraction time=5min, no salt addition to sample, type and volume of the eluent=50μL methanol, and desorption time=1min. Under the optimum conditions detection limits and linear dynamic ranges were achieved in the range of 1.8-3.0, 5-1500μgL(-1) for DPH and 1.5-3.5, 5-1500μgL(-1) for DIC, respectively. The percent of extraction recovery and relative standard deviations (n=5) were in the range of 47.3-60, 5.2-9.0 for DPH and 64-76.7, 5.1-5.8 for DIC, respectively. Ultimately, the applicability of the method was successfully confirmed by the extraction and determination of DIC and DPH in human urine, plasma and waste water samples in the range of microgram per liter and satisfactory results were obtained.
在样品制备策略中,从不同样品中共萃取酸性和碱性药物是一个备受关注且存在争议的概念。在本研究中,首次引入了基于磁性纳米颗粒的分散微固相萃取结合高效液相色谱 - 紫外检测法同时萃取酸性和碱性药物。十六烷基三甲基溴化铵包覆的Fe₃O₄@癸酸作为一种高效吸附剂,成功应用于吸附双氯芬酸(DIC)作为酸性模型化合物和苯海拉明(DPH)作为碱性模型化合物。首先,将适量合成的Fe₃O₄@癸酸纳米颗粒加入到药物水溶液中。调节溶液pH后,将十六烷基三甲基溴化铵(CTAB)加入到以恒定速率搅拌的混合物中。药物吸附并通过磁场倾析上清液后,用甲醇剧烈涡旋洗脱吸附剂。优化了影响萃取效率的参数,得到:样品pH = 9,CTAB浓度 = 0.2mmolL⁻¹,吸附剂用量 = 10mg,萃取时间 = 5min,样品不添加盐,洗脱剂类型和体积 = 50μL甲醇,解吸时间 = 1min。在最佳条件下,DPH的检测限和线性动态范围分别为1.8 - 3.0、5 - 1500μgL⁻¹,DIC的检测限和线性动态范围分别为1.5 - 3.5、5 - 1500μgL⁻¹。DPH的萃取回收率百分比和相对标准偏差(n = 5)分别在47.3 - 60、5.2 - 9.0范围内,DIC的萃取回收率百分比和相对标准偏差(n = 5)分别在64 - 76.7、5.1 - 5.8范围内。最终,通过在微克每升范围内对人尿液、血浆和废水样品中的DIC和DPH进行萃取和测定,成功证实了该方法的适用性,并获得了满意的结果。