Li Xiao, Chen Jia, Li Xuanwei, Xia Yaokun, Zhao Qingwei
Department of Clinical Pharmacy, The First Affiliated Hospital, Zhejiang University School of Medicine, Hangzhou, 310003, China.
Zhejiang Provincial Key Laboratory for Drug Evaluation and Clinical Research, Hangzhou, 310003, China.
Anal Bioanal Chem. 2025 Jul 21. doi: 10.1007/s00216-025-06016-6.
A dispersive liquid-liquid microextraction method based on high-density alkanol-hexafluoroisopropanol supramolecular solvent (alkanol-HFIP SUPRAS) coupled with liquid chromatography-tandem mass spectrometry is presented for microextraction and detection of four antipsychotics (aripiprazole, lurasidone, risperidone, and paliperidone) in urinary specimens. With octanol as the extractant and HFIP as the dispersant, SUPRAS-forming agent, and density regulator, reverse micelle aggregate-based SUPRAS spontaneously formed in urine, which acted as SUPRAS inducer and analytical sample. SUPRAS formation was not limited by sample pH or salt addition. The SUPRAS, located at the bottom layer of the sample solution due to its high density, was easily collected in trace volumes (~14 μL). Extraction conditions were studied and screened by the one-variable-at-a-time method, the Box-Behnken design, and response surface modeling. Optimal conditions provided low solvent consumption (70 μL of octanol and HFIP), short extraction time (40 s of vortex time), high extraction rate (61-78%), and good enrichment factor (44-55). There is a good linear relationship with correlation coefficients higher than 0.9959. Method limits of detection (S/N = 3) and quantification (S/N = 10) were in the ranges of 0.13-0.38 ng mL and 0.42-1.28 ng mL, respectively. Recoveries ranged from 94.0 to 120.3% with intra- and inter-day relative standard deviations less than 9.9%. The method also has satisfactory levels of eco-friendliness and sustainability (0.56 of AGREEprep score) with low matrix effects (87.4-113.0%). The method is a fast, simple, efficient, and environmentally benign procedure for microextraction and detection of antipsychotics in human urine.
本文提出了一种基于高密度链烷醇 - 六氟异丙醇超分子溶剂（链烷醇 - HFIP SUPRAS）结合液相色谱 - 串联质谱法的分散液 - 液微萃取方法，用于尿液样本中四种抗精神病药物（阿立哌唑、鲁拉西酮、利培酮和帕利哌酮）的微萃取和检测。以正辛醇为萃取剂，HFIP为分散剂、超分子溶剂形成剂和密度调节剂，基于反胶束聚集体的SUPRAS在尿液中自发形成，其作为SUPRAS诱导剂和分析样品。SUPRAS的形成不受样品pH值或加盐的限制。由于其高密度，SUPRAS位于样品溶液的底层，易于以微量体积（约14μL）收集。通过单变量法、Box - Behnken设计和响应面建模研究并筛选了萃取条件。最佳条件下溶剂消耗低（70μL正辛醇和HFIP）、萃取时间短（涡旋时间40秒）、萃取率高（61 - 78%）且富集因子良好（44 - 55）。具有良好的线性关系，相关系数高于0.9959。方法检测限（S/N = 3）和定量限（S/N = 10）分别在0.13 - 0.38 ng/mL和0.42 - 1.28 ng/mL范围内。回收率在94.0%至120.3%之间，日内和日间相对标准偏差小于9.9%。该方法还具有令人满意的生态友好性和可持续性水平（AGREEprep评分0.56），基质效应低（87.4 - 113.0%）。该方法是一种快速、简单、高效且环境友好的用于人尿中抗精神病药物微萃取和检测的方法。
