Key Laboratory of Nanobiosensing and Nanobioanalysis at Universities of Jilin Province, Department of Chemistry, Northeast Normal University, 5268 Renmin Street, Changchun, Jilin Province 130024, PR China.
Key Laboratory of Nanobiosensing and Nanobioanalysis at Universities of Jilin Province, Department of Chemistry, Northeast Normal University, 5268 Renmin Street, Changchun, Jilin Province 130024, PR China.
Talanta. 2018 Apr 1;180:90-97. doi: 10.1016/j.talanta.2017.12.035. Epub 2017 Dec 15.
A tapered-capillary microextraction (tCap-μEx) combining with field-amplified stacking (FASI) method for CE analysis was developed. The tCap-μEx method is based on the construction of a micro solid phase extraction (SPE) column by narrowing the end of a silica capillary from 530µm (inner diameter) to 20µm, enabling the packing of 45µm sorbent particles without a frit. Various parameters that may affect the microextraction and FASI-CE analysis have been investigated and optimized. This study shows that microextraction exhibits advantages of small sample and sorbent volumes (less than 200μL sample and 2μL sorbent) and fast extraction time of 6min. The method was successfully applied for efficient determination of atenolol and metoprolol in human urine samples, with recovery of 93.7-105.5% and RSD (n=3) lower than 8.5%. Twenty-one-fold and nineteen-fold average enhancement of detection sensitivity was achieved for atenolol and metoprolol, respectively, versus the CE method without tCap-μEx and FASI. The method is environmentally friendly and allows reuse of the sorbent at least 8 times without an obvious loss in performance. The results indicate that the proposed method could be potentially applied in a wide range of doping control, clinical, forensic toxicology, food analysis and environmental analyses.
一种基于锥形毛细微萃取（tCap-μEx）结合场放大堆积（FASI）的毛细管电泳分析方法被开发出来。tCap-μEx 方法是基于从 530µm（内径）缩小到 20µm 的硅毛细管末端构建微型固相萃取（SPE）柱，实现了无需 frit 的 45µm 吸附剂颗粒的填充。已经研究和优化了可能影响微萃取和 FASI-CE 分析的各种参数。本研究表明，微萃取具有小样品和吸附剂体积（小于 200µL 样品和 2µL 吸附剂）以及 6min 快速萃取时间的优势。该方法成功应用于人体尿液中阿替洛尔和美托洛尔的高效测定，回收率为 93.7-105.5%，RSD（n=3）低于 8.5%。与没有 tCap-μEx 和 FASI 的 CE 方法相比，阿替洛尔和美托洛尔的检测灵敏度分别提高了 21 倍和 19 倍。该方法环保，允许至少重复使用 8 次吸附剂，而不会明显降低性能。结果表明，该方法可广泛应用于兴奋剂检测、临床、法医毒理学、食品分析和环境分析等领域。
