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Multivariate Optimization of an Ultrasound-Assisted Deep Eutectic Solvent-Based Liquid-Phase Microextraction Method for HPLC–UV Analysis of Carbamazepine in Plasma
Chromatographia ( IF 1.7 ) Pub Date : 2020-09-28 , DOI: 10.1007/s10337-020-03966-0
Hassan Heidari , Boshra Yari

An ultrasound-assisted deep eutectic solvent-based liquid-phase microextraction (UA-DES-LPME) was established, for the first time, for the extraction of carbamazepine (CBZ) from human plasma samples. The extract was determined by HPLC-ultraviolet detection (HPLC–UV). A deep eutectic solvent (DES) was readily synthesized by mixing choline chloride and phenol (ChCl:Ph) in the mole ratio of 1:2 in ambient temperature and used without any further purification. In the present method, THF was used as an emulsifier agent. Some parameters, including the DES components mole ratio, kind of emulsifier agent, and salt addition effect, were optimized by a one-at-a-time approach. Central composite design (CCD) was used to optimize the rest of the effective parameters, including DES volume, pH, ultrasonication time, and THF volume. The optimum conditions were found to be: 11.78 pH, 314 µL DES volume, 523 µL THF volume, and 9.0 min ultrasonication time. The performance of the method was evaluated under optimum conditions, and the method exhibited good linearity over a concentration range of 10–1500 ng mL−1, low limit of detection and quantitation, good precision, and high extraction recovery. Finally, the applicability of the method was assessed by analysis of the spiked plasma samples, and the results have shown high relative recoveries with good precision.

中文翻译:

用于血浆中卡马西平 HPLC-UV 分析的超声辅助深共晶溶剂液相微萃取方法的多变量优化

首次建立了超声辅助深共晶溶剂型液相微萃取(UA-DES-LPME),用于从人血浆样品中提取卡马西平(CBZ)。提取物通过 HPLC-紫外检测 (HPLC-UV) 测定。通过在环境温度下以 1:2 的摩尔比混合氯化胆碱和苯酚 (ChCl:Ph) 很容易合成一种深共熔溶剂 (DES),并且无需任何进一步纯化即可使用。在本方法中,THF用作乳化剂。一些参数,包括 DES 组分摩尔比、乳化剂的种类和加盐效果,通过一次一个的方法进行优化。中心复合设计 (CCD) 用于优化其余有效参数,包括 DES 体积、pH、超声处理时间和 THF 体积。发现最佳条件为:11.78 pH、314 µL DES 体积、523 µL THF 体积和 9.0 分钟超声处理时间。在最佳条件下对该方法的性能进行了评估,该方法在 10-1500 ng mL-1 的浓度范围内表现出良好的线性,检测和定量限低,精密度好,提取回收率高。最后,通过分析加标血浆样品来评估该方法的适用性,结果显示相对回收率高且精密度好。和高提取回收率。最后,通过对加标血浆样品的分析来评估该方法的适用性,结果显示出较高的相对回收率和良好的精密度。和高提取回收率。最后,通过对加标血浆样品的分析来评估该方法的适用性,结果显示出较高的相对回收率和良好的精密度。
更新日期:2020-09-28
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