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<p>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&#xa0;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&#xa0;ng&#xa0;mL<sup>−1</sup> and 0.42–1.28&#xa0;ng&#xa0;mL<sup>−1</sup>, 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.</p>

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Alkanol–hexafluoroisopropanol high-density supramolecular solvent-based dispersive liquid–liquid microextraction of antipsychotics in human urine

  • 期刊论文

  • 发表日期：

    2025年7月21日

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  • Xiao Li,
  • Jia Chen,
  • Xuanwei Li,
  • Yaokun Xia,
  • Qingwei Zhao

摘要

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−1 and 0.42–1.28 ng mL−1, 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.