Mohammad Nejad Leila, Pashaei Yaser, Daraei Bahram, Forouzesh Mehdi, Shekarchi Maryam
Department of Toxicology, Faculty of Medical Sciences, Tarbiat Modares University Tehran, Iran.
Young Researchers and Elite Club, Tehran Medical Sciences, Islamic Azad University, Tehran, Iran.
Iran J Pharm Res. 2019 Spring;18(2):642-657. doi: 10.22037/ijpr.2019.1100676.
In this work, a reusable graphene oxide (GO) based dispersive-solid phase extraction (d-SPE) was synthesized and used for the analysis of trace ampicillin sodium (AMP) and clindamycin hydrochloride (CLI) in water samples followed by high performance liquid chromatography-UV detection (HPLC-UV). Batch experiments were conducted to investigate the effects of pH and volume of the sample solution, contact time, adsorption isotherms, temperature, and desorption conditions. The maximum adsorption capacities of AMP and CLI on GO nanosheets were found to be 33.33 mg g and 47 mg g, respectively. The adsorption isotherm data can be well fitted by Temkin (AMP and CLI) and Freundlich (AMP), and the adsorption process followed the pseudo-second-order model. The thermodynamic parameters were calculated, indicated that the adsorption process of both analytes were spontaneous and exothermic. In addition, the d-SPE following HPLC analyses showed good linearity in the range of 0.5-200 ng mL (R= 0.999) for AMP and 1-200 ng mL (R= 0.999) for CLI, with LOD of 0.04 and 0.24 ng mL for AMP and CLI, respectively. The percent of extraction recoveries, intra and inter-day precisions (expressed as RSD %, n = 3) were in the range of 96.4-101.6%, 2.2-3.0, and 3.7-4.7 for AMP as well as 94.2-98.6%, 2.2-3.8, and 3.5-4.6 for CLI, respectively. The preconcentration factor of 20 was achieved for both analytes. From these results, it can be concluded that the validated method is a simple, cost-effective and repeatable method for analysis of AMP and CLI in water samples and provide a new platform for antibiotics decontamination.
在本研究中,合成了一种基于氧化石墨烯(GO)的可重复使用的分散固相萃取(d-SPE)材料,并将其用于水样中痕量氨苄西林钠(AMP)和盐酸克林霉素(CLI)的分析,随后采用高效液相色谱-紫外检测(HPLC-UV)法。进行了批量实验,以研究样品溶液的pH值、体积、接触时间、吸附等温线、温度和解吸条件的影响。发现AMP和CLI在GO纳米片上的最大吸附容量分别为33.33 mg/g和47 mg/g。吸附等温线数据能很好地用Temkin模型(AMP和CLI)和Freundlich模型(AMP)拟合,吸附过程遵循准二级模型。计算了热力学参数,表明两种分析物的吸附过程都是自发的且放热。此外,HPLC分析后的d-SPE法对AMP在0.5-200 ng/mL范围内(R=0.999)以及对CLI在1-200 ng/mL范围内(R=0.999)显示出良好的线性,AMP和CLI的检出限分别为0.04和0.24 ng/mL。AMP的萃取回收率、日内和日间精密度(以RSD%表示,n = 3)分别在96.4-101.6%、2.2-3.0和3.7-4.7范围内,CLI的分别在94.2-98.6%、2.2-3.8和3.5-4.6范围内。两种分析物的预富集因子均达到20。从这些结果可以得出结论,该验证方法是一种简单、经济高效且可重复的分析水样中AMP和CLI的方法,并为抗生素去污提供了一个新平台。