Moghadam Ahmad Ghoochani, Rajabi Maryam, Asghari Alireza
Department of Chemistry, Semnan University, Semnan 2333383-193, Iran.
Department of Chemistry, Semnan University, Semnan 2333383-193, Iran.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Jan 1;1072:50-59. doi: 10.1016/j.jchromb.2017.09.042. Epub 2017 Sep 28.
In this research work, an efficient, facile, prompt, and relatively safe enrichment procedure, named as air agitated-emulsification microextraction based on a low density-deep eutectic solvent (AA-EME-LD-DES), was applied for the first time to separate trace amounts of the drugs escitalopram, desipramine, and imipramine from complex sample solutions. This bio-degradable and cheap choline chloride-based extracting agent was readily prepared by the easy blending process at the ambient temperature, resulting in a eutectic liquid mixture with distinct features. Also the subsequent usage of an effective proceeding of the current microextraction procedure without a vital requirement for a further purification was adopted as another impressive benefit. Investigation of the main parameters influencing the multivariate technique based on the central composite design (CCD) combined with the desirability function (DF) revealed that pH12.0, 200μL of the extraction solvent, 430μL of the emulsifier solvent, and 14 air agitation cycles led to maximum extraction efficiencies with the DF value close to 0.97. Under the optimal experimental conditions, the wide linear dynamic ranges (LDRs) of 10.0-5000, 15.0-8000, and 15.0-6000ngmL for escitalopram, desipramine, and imipramine were accurately obtainable, respectively, with the determination coefficients (Rs) higher than 0.98 and the low limits of detection (LODs) of 3.0-4.5ngmL. The percent extraction recoveries and enrichment factors were found to be adequately quantitative in the spans of 42-68% and 25-40, respectively, possessing good relative standard deviations (%RSDs, n=3) in the range of 3.6-5.7%. Finally, accurate analyses at therapeutically low ranges for the human plasma sample and trace levels for the pharmaceutical wastewater sample were successfully obtained, certifying the appropriate pre-concentration and enrichment capabilities of the proposed microextraction approach.
在本研究工作中,首次应用了一种高效、简便、快速且相对安全的富集方法,即基于低密度-深共熔溶剂的空气搅拌-乳化微萃取(AA-EME-LD-DES),从复杂样品溶液中分离痕量的艾司西酞普兰、地昔帕明和丙咪嗪。这种可生物降解且廉价的基于氯化胆碱的萃取剂在室温下通过简单混合过程即可轻松制备,得到具有独特特性的共熔液体混合物。此外,当前微萃取程序后续使用时无需进一步纯化这一有效步骤,这也是另一个显著优点。基于中心复合设计(CCD)结合可取性函数(DF)对影响多变量技术的主要参数进行研究表明,pH 12.0、200μL萃取溶剂、430μL乳化剂溶剂和14次空气搅拌循环可实现最大萃取效率,DF值接近0.97。在最佳实验条件下,艾司西酞普兰、地昔帕明和丙咪嗪的宽线性动态范围(LDRs)分别准确可达10.0 - 5000、15.0 - 8000和15.0 - 6000 ng/mL,测定系数(Rs)高于0.98,检测下限(LODs)为3.0 - 4.5 ng/mL。萃取回收率和富集因子在42 - 68%和25 - 40范围内分别具有足够的定量性,相对标准偏差(%RSDs,n = 3)在3.6 - 5.7%范围内。最后,成功获得了人血浆样品治疗低浓度范围和制药废水样品痕量水平的准确分析结果,证明了所提出的微萃取方法具有适当的预浓缩和富集能力。