Evaluation of sample preparation and chromatographic separation for the parallel determination of taurine and edaravone in rat tissues using HILIC-MS/MS.

The quantitative analysis of taurine and edaravone in biological sample is critical in pharmaceutical studies. Although each of them can be individually analyzed by different approaches, concurrent quantification is still a highly challenging task with respect to their great polarity variation and the complex composition of tissue sample. In the present study, to simultaneously determine taurine and edaravone in rat tissue, the sample preparation and chromatographic separation conditions were evaluated and discussed in detail. As for the sample preparation, four kinds of solvent and the volume ratio of the optimal solvent to biological sample were both tested and evaluated based on the chromatographic profile, extraction recovery, and matrix effect (ME). The chromatographic separation was performed in a reverse phase (RP) and two hydrophilic interaction liquid chromatography (HILIC) modes, and the corresponding separation efficiencies were assessed using chromatographic parameters like half-width (W 1/2 ), tailing factor (f t), theoretical plates number (N), and ME. Furthermore, adopted composition of two mobile phase systems and the concentrations of the additives in the optimum buffer system were also investigated on an Atlantis HILIC silica column according to the resultant chromatographic profiles and peak areas of the analytes. The optimal results were obtained when the biological samples were deproteined by 4-fold volume of methanol/acetonitrile (1:3, v/v) and separated on a HILIC column with a gradient elution of acetonitrile/water containing 0.2 % formic acid and 10 mM ammonium formate. The proposed approach was validated and successfully applied to the parallel determination of the tissue distribution of edaravone and taurine in rat tissues.

Occurrence and source analysis of selected antidepressants and their metabolites in municipal wastewater and receiving surface water.

Seven commonly utilized antidepressants (amitriptyline, fluoxetine, sertraline, citalopram, paroxetine, venlafaxine, and bupropion) and three of their metabolites were detected in four wastewater treatment plants (WWTPs) and corresponding receiving waters including the mainstream and three of the tributaries of Huangpu River, Shanghai. The concentration levels of selected antidepressants in wastewater and receiving water were both at ng L-1 level, but those antidepressants that were found in wastewater were typically in a range of one and even two orders of magnitude higher than those that were present in the receiving water except for the concentration levels of paroxetine, norfluoxetine, and nortriptyline. Venlafaxine and its metabolite O-desmethylvenlafaxine were the primary compounds (reaching up to 132.04 and 173.68 ng L-1 as well as 3.03 and 4.53 ng L-1 in wastewater and receiving water, respectively). Based on the mass loadings of selected antidepressants in four WWTPs, the mass loading of sertraline in effluent for this study was at the highest level when compared to other countries. The important finding was that the sampling sites H11 and H13 were much more likely to be polluted by side-pollution sources (the accumulation areas of Grade A of Class-three hospitals and pharmaceutical factories) than point pollution sources (WWTP 1 and WWTP2) through analysis of Spearman correlation. The results have shown that the RQs for these antidepressants were less than 0.1 except for the RQ of venlafaxine in an effluent for mollusks, which was less than 1. This indicated that the concentration levels of antidepressants would not pose a high risk for aquatic organisms, but sustained attention should still be paid.