Department of Chemistry, National Kaohsiung Normal University, Taiwan.
Department of Chemistry, National Kaohsiung Normal University, Taiwan.
J Chromatogr A. 2023 Aug 30;1705:464212. doi: 10.1016/j.chroma.2023.464212. Epub 2023 Jul 13.
In this study, a simple, rapid, and ultrasensitive technique was developed to identify five pairs of phenothiazine drugs by using ultrasound-enhanced and surfactant-assisted dispersive liquid-liquid microextraction (UESA-DLLME), field-amplified sample injection with capillary electrophoresis (FASI-CE), and capacitively coupled capacitively coupled contactless conductivity detection (CD). During the CE separation process, UESA-DLLME was used for sample clean-up and offline concentration, and FASI-CE was used for the online concentration of phenothiazine enantiomers. At baseline, the five pairs of phenothiazine enantiomer drugs required 18 min for separation. UESA-DLLME was then used to extract 0.01 mM Tween 80 at pH 10 from a sample solution (extraction solvent, 100 mL of dichloromethane). Subsequently, FASI was used to stack the sample solution (buffer, 30 mM 2-(N-morpholino)ethanesulfonic acid/aspartic acid, additive 4 mM hydroxypropyl-γ-cyclodextrin, pH 2.5), and CD was used for signal detection (amplitude, 2 Vpp; frequency, 400 kHz). The results indicated that the linear range for quantifying all analyte enantiomers was 1.0-150 nM, with a coefficient of determination exceeding 0.99. In addition, the relative standard deviations in the migration time and peak areas for the 10 analytes were less than 3.2% and 7.2%, respectively. The proposed system has a limit of detection (LOD) for the 10 analytes at a signal-to-noise ratio of 3, ranging from 0.24 to 0.28 nM. The sensitivity enhancement, which compares the LOD (limit of detection in the normal method) to LOD (limit of detection achieved using the proposed UESA-DLLME-FASI-CE-CD method), varies between approximately 1200 and 2000 for the 10 analytes. Analysis of the 10 separated analytes spiked in urine and serum samples revealed recovery rates of 88%-106% and 89%-105%, respectively. Therefore, this highly sensitive advanced technique was successfully used to analyze phenothiazine enantiomers in urine and serum samples.
在这项研究中，开发了一种简单、快速、超灵敏的技术，通过超声增强和表面活性剂辅助分散液-液微萃取（UESA-DLLME）、场放大样品进样与毛细管电泳（FASI-CE）和电容耦合非接触式电导检测（CD）来识别五对吩噻嗪类药物。在 CE 分离过程中，UESA-DLLME 用于样品净化和离线浓缩，而 FASI-CE 用于吩噻嗪对映体的在线浓缩。在基线处，五对吩噻嗪对映体药物需要 18 分钟才能分离。然后使用 UESA-DLLME 从样品溶液（提取溶剂，100 mL 二氯甲烷）中提取 0.01 mM Tween 80。随后，使用 FASI 对样品溶液（缓冲液，30 mM 2-（N-吗啉基）乙磺酸/天冬氨酸，添加剂 4 mM 羟丙基-γ-环糊精，pH 2.5）进行堆积，使用 CD 进行信号检测（幅度，2 Vpp；频率，400 kHz）。结果表明，定量所有分析物对映体的线性范围为 1.0-150 nM，相关系数均大于 0.99。此外，10 种分析物的迁移时间和峰面积的相对标准偏差均小于 3.2%和 7.2%。对于 10 种分析物，该系统的检出限（LOD）在信噪比为 3 时为 0.24-0.28 nM。灵敏度增强，将 10 种分析物的检出限（正常方法的检出限）与检出限（使用提议的 UESA-DLLME-FASI-CE-CD 方法获得的检出限）进行比较，在 10 种分析物之间的变化范围为 1200 至 2000 倍。对尿液和血清样品中添加的 10 种分离分析物的分析表明，回收率分别为 88%-106%和 89%-105%。因此，该高灵敏度先进技术成功用于分析尿液和血清样品中的吩噻嗪对映体。
