School of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006, China; Nano Diagnosis for Health Biotech (Guangzhou) Co., Ltd., Guangzhou 510535, China.
Anti-Drug Technology Center of Guangdong Province, Guangdong Provincial Key Laboratory of Psychoactive Substances Monitoring and Safety, Guangzhou 510230, China.
Ecotoxicol Environ Saf. 2023 Sep 15;263:115302. doi: 10.1016/j.ecoenv.2023.115302. Epub 2023 Jul 26.
A novel method for simultaneous separation and detection of the racemates and the enantiomers of common chiral antidepressants in wastewater matrix was developed by online heart-cutting two-dimensional liquid chromatography (2D-LC) coupled to solid-phase extraction (SPE). Screening of chiral stationary phases (CSPs) and chromatographic conditions was investigated for complete enantioseparation to be compatible with RP-HPLC in 1st D-LC. Using methanol-0.1 % (v/v) ammonia solution as mobile phase, a 2D-LC system was configured by reversed mode with a combination of C18 column and the serially CPS columns as 2D-LC stationary phases respectively. The target analytes could achieve satisfactory transformation between 2D-LCs with transfer rate of 90.57-98.58 %. By means of freeze-drying and SPE, three antidepressants in wastewater were greatly preconcentrated under the optimized conditions, improving the method performance. The racemates and the enantiomers of mirtazapine, bupropion and fluoxetine exhibited good linearity in the range of 0.10-30.00 ng/mL (R≥0.9986), and LODs and LOQs ranged in 0.0183-0.0549 ng/mL and 0.0661-0.1831 ng/mL, respectively. By this way, the method was successfully applied to simultaneous determination of the racemates and the enantiomers of mirtazapine, bupropion and fluoxetine in wastewater samples. Among them, three samples contained bupropion at level of 0.401-0.822 ng/mL, and mirtazapine at level of 0.328 and fluoxetine at level of 0.381 ng/mL were detected respectively in the other two samples. The enantiomers were at level of 0.140-0.189 ng/mL for mirtazapine, 0.182-0.419 ng/mL for bupropion and 0.179-0.204 ng/mL for fluoxetine, respectively. The proposed method providing an efficient approach to monitoring chiral drugs and their enantiomers in wastewater, facilitating to pollution assessment of chiral drugs in the environment and regional survey of illicit abuse in drug control.
建立了一种新颖的方法,用于通过在线心切割二维液相色谱(2D-LC)与固相萃取(SPE)联用,同时分离和检测废水中常见手性抗抑郁药对映体和外消旋体。本文筛选了手性固定相(CSP)并优化了色谱条件,以实现完全对映体分离,并与 1D-LC 中的反相高效液相色谱(RP-HPLC)兼容。使用甲醇-0.1%(v/v)氨溶液作为流动相,通过反相模式配置 2D-LC 系统,分别使用 C18 柱和串联 CSP 柱作为 2D-LC 固定相。在优化条件下,通过冷冻干燥和 SPE,三种抗抑郁药在废水中得到了极大的预浓缩,提高了方法性能。米氮平、安非他酮和氟西汀的对映体和外消旋体在 0.10-30.00ng/mL 范围内表现出良好的线性关系(R≥0.9986),检出限和定量限范围分别为 0.0183-0.0549ng/mL 和 0.0661-0.1831ng/mL。该方法成功应用于废水中米氮平、安非他酮和氟西汀对映体和外消旋体的同时测定。其中,三个样品中安非他酮的含量为 0.401-0.822ng/mL,另外两个样品中米氮平的含量为 0.328ng/mL,氟西汀的含量为 0.381ng/mL。对映体的含量分别为米氮平 0.140-0.189ng/mL,安非他酮 0.182-0.419ng/mL,氟西汀 0.179-0.204ng/mL。该方法为监测废水中手性药物及其对映体提供了一种有效的方法,有助于对手性药物在环境中的污染评估和药物管制中非法滥用的区域调查。