Department of Chemistry, National Kaohsiung Normal University, Kaohsiung, Taiwan.
Division of Gastroenterology and Hepatology, Department of Medicine, Kaohsiung Veterans General Hospital, Kaohsiung, Taiwan.
J Sep Sci. 2018 Apr;41(8):1871-1879. doi: 10.1002/jssc.201701096. Epub 2018 Feb 9.
A new version of dispersive liquid-liquid microextraction, namely, cyclodextrin-assisted dispersive liquid-liquid microextraction, with subsequent sweeping micellar electrokinetic chromatography has been developed for the preconcentration and sensitive detection of carbamazepine and clobazam. α-Cyclodextrin and chloroform were used as the dispersive agent and extraction solvent, respectively. After the extraction, carbamazepine and clobazam were analyzed using micellar electrokinetic chromatography with ultraviolet detection. The detection sensitivity was further enhanced using the sweeping technique. Under optimal extraction and stacking conditions, the calibration curves of carbamazepine and clobazam were linear over a concentration range of 2.0-200.0 ng/mL. The method detection limits at a signal-to-noise ratio of 3 were 0.6 and 0.5 ng/mL with sensitivity enhancement factors of 3575 and 4675 for carbamazepine and clobazam, respectively. This developed method demonstrated high sensitivity enhancement factors and was successfully applied to the determination of carbamazepine and clobazam in human urine samples. The precision and accuracy for urine samples were less than 4.2 and 6.9%, respectively.
一种新的分散液-液微萃取方法，即环糊精辅助分散液-液微萃取，随后采用胶束电动色谱进行扫集，用于卡马西平和氯硝西泮的预浓缩和灵敏检测。α-环糊精和氯仿分别用作分散剂和萃取溶剂。萃取后，采用胶束电动色谱法结合紫外检测分析卡马西平和氯硝西泮。采用扫集技术进一步提高了检测灵敏度。在最佳萃取和堆积条件下，卡马西平和氯硝西泮的校准曲线在 2.0-200.0ng/mL 的浓度范围内呈线性。在信噪比为 3 时，卡马西平和氯硝西泮的方法检测限分别为 0.6 和 0.5ng/mL，卡马西平和氯硝西泮的灵敏度增强因子分别为 3575 和 4675。所开发的方法具有高的灵敏度增强因子，并成功应用于人尿样中卡马西平和氯硝西泮的测定。尿样的精密度和准确度分别小于 4.2%和 6.9%。
