Department of Pharmaceutical Chemistry, Medical University of Gdańsk, Hallera 107, 80-416 Gdańsk, Poland.
Department of Pharmaceutical Chemistry, Medical University of Gdańsk, Hallera 107, 80-416 Gdańsk, Poland.
Anal Chim Acta. 2014 Feb 6;811:88-93. doi: 10.1016/j.aca.2013.12.021. Epub 2013 Dec 26.
A field-amplified sample injection (FASI) technique was elaborated for fast and sensitive determination of selected central nervous system drugs in human urine samples. Factors affecting the sensitivity enhancement, such as background electrolyte (BGE) and the analytical matrix composition were optimized and discussed. Pseudo-isotachophoresis (p-ITP) mechanism contribution in preconcentration mechanism was discussed. All separations were performed in uncoated fused silica capillaries 50 μm × 57 cm at 22 kV. The optimized analytical matrix was composed of 0.25 mM HCOOH in 90% (v/v) methanol, while BGE contained 45 mM TRIS/HCl (pH 2.20). The head-column injection was performed in 0.25 mM HCOOH water solution (3s, 3.45 kPa). Sample was introduced into the capillary by electrokinetic injection (70 s, 5 kV) followed by short BGE plug (3s, 3.45 kPa). Seven psychiatric drugs (olanzapine, prochlorperazine dimaleate, trifluoperazine dihydrochloride, perphenazine, promazine hydrochloride, clomipramine hydrochloride, and chlorprothixene hydrochloride) were separated in about 6 min. The elaborated method was additionally supported with dispersive liquid-liquid microextraction (DLLME) technique which in summary with FASI provided about 8000-13,000-fold sensitivity enhancement in comparison to the capillary zone electrophoresis (CZE) method with standard hydrodynamic injection (5s, 3.45 kPa).
一种场放大样品进样（FASI）技术被详细阐述，用于快速灵敏地测定人尿样中的选定中枢神经系统药物。讨论了影响灵敏度增强的因素，如背景电解质（BGE）和分析基质组成。讨论了伪等速电泳（p-ITP）机制在浓缩机制中的贡献。所有分离均在未涂层熔凝硅毛细管（50 μm × 57 cm）中在 22 kV 下进行。优化的分析基质由 0.25 mM HCOOH 在 90%（v/v）甲醇中组成，而 BGE 包含 45 mM TRIS/HCl（pH 2.20）。柱头进样在 0.25 mM HCOOH 水溶液中进行（3s，3.45 kPa）。样品通过电动进样（70 s，5 kV）引入毛细管，随后是短 BGE 塞（3s，3.45 kPa）。七种精神药物（奥氮平、丙氯拉嗪马来酸盐、三氟拉嗪二盐酸盐、奋乃静、丙嗪盐酸盐、氯米帕明盐酸盐和氯普噻吨盐酸盐）在大约 6 分钟内分离。该方法还辅以分散液-液微萃取（DLLME）技术，与 FASI 相结合，与标准水力进样的毛细管区带电泳（CZE）方法相比，灵敏度提高了约 8000-13000 倍。
