Qin Yaxin, Gao Wei, Xu Jian, Ping Li, Tong Shengqiang, Liu Biao, Chu Chu
College of Pharmaceutical Science, Zhejiang University of Technology, Hangzhou, PR China.
Center for Drug Safety Evaluation and Research of Zhejiang University, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou, PR China.
Anal Chim Acta. 2024 Jul 4;1311:342736. doi: 10.1016/j.aca.2024.342736. Epub 2024 May 16.
Capillary electrophoresis is a powerful analytical method featured with high separation efficiency, minimal sample requirements, and reduced organic solvents consumption. However, its low sensitivity hinders its wide application in determination of trace analytes especially for the weakly ionized hydrophobic compounds. Offline and Online capillary electrophoresis stacking methods are more favored to enhance detection sensitivity of analytes. The determination of two sesquiterpenes and an alkaloid from the dried root of Lindera aggregata merged as an example for developing a simple, sensitive and green method for the simultaneous determination of two hydrophobic compounds in complicated matrix samples.
An offline-online capillary electrophoresis stacking strategy by integrating micro matrix solid phase dispersion with field-amplified sample stacking and micelle to cyclodextrin stacking has been developed for the simultaneous determination of dehydrocostus lactone, linderane, norisoboldine in complex matrices. The optimized parameters were set at 65 mM sodium dihydrogen phosphate, 35 % methanol, 180 s for sample injection and 210 s for cyclodextrin injection, 20 mM sodium dodecyl sulfate of sample matrix for online stacking; 1:1 sample to MCM-48, 180 s grinding time, and 1000 μL of 20 mM sodium dodecyl sulfate elution for offline procedure. Under the optimum conditions, the method showed good linearity with correlation coefficients (R ≥ 0.9927), low limits of detection within the range of 25-50 ng mL, satisfactory repeatability and reproducibility below 3.98 %, and acceptable recoveries between 94 % and 97 %. The developed method was successfully applied to two real samples, the root of L. aggregata and rat feces.
Sodium dodecyl sulfate is firstly used as an eluent in micro matrix solid phase dispersion and plays a dual role throughout the analytical procedure, including extraction solvent in sample preparation and micelle pseudophase during online stacking. It brings great procedure convenience to the method. The sensitivity of this method can improve up to 1283-folds compared with the normal mode. Moreover, the overall strategy indicates satisfied green potential evaluated by greenness assessment tools.
毛细管电泳是一种强大的分析方法,具有分离效率高、样品需求量少和有机溶剂消耗低等特点。然而,其低灵敏度阻碍了它在痕量分析物测定中的广泛应用,尤其是对于弱电离的疏水化合物。离线和在线毛细管电泳堆积方法更有利于提高分析物的检测灵敏度。以乌药干燥根中两种倍半萜和一种生物碱的测定为例,开发一种简单、灵敏且绿色的方法,用于同时测定复杂基质样品中的两种疏水化合物。
建立了一种离线-在线毛细管电泳堆积策略,该策略将微基质固相分散与场放大进样堆积和胶束-环糊精堆积相结合,用于同时测定复杂基质中的脱氢木香内酯、乌药醚内酯、去甲异波尔定。优化参数设定为:65 mM磷酸二氢钠、35%甲醇、进样180 s、环糊精进样210 s、在线堆积时样品基质为20 mM十二烷基硫酸钠;离线过程中,样品与MCM-48比例为1:1、研磨时间180 s、用1000 μL 20 mM十二烷基硫酸钠洗脱。在最佳条件下,该方法线性良好,相关系数(R≥0.9927),检测限低,在25 - 50 ng/mL范围内,重复性和重现性良好,低于3.98%,回收率在94%至97%之间。所开发的方法成功应用于两个实际样品,即乌药根和大鼠粪便。
十二烷基硫酸钠首次用作微基质固相分散的洗脱剂,在整个分析过程中发挥双重作用,包括样品制备中的萃取溶剂和在线堆积时的胶束假相。这给该方法带来了极大的操作便利性。与常规模式相比,该方法的灵敏度可提高至1283倍。此外,通过绿色度评估工具评估,整体策略显示出良好的绿色潜力。