Centro de Química Estrutural, Faculdade de Ciências, Universidade de Lisboa, Campo Grande, 1749-016 Lisboa, Portugal.
Departamento de Química e Bioquímica, Faculdade de Ciências, Universidade de Lisboa, Campo Grande, 1749-016 Lisboa, Portugal.
Molecules. 2020 Mar 22;25(6):1438. doi: 10.3390/molecules25061438.
We developed, optimized and validated a fast analytical cycle using high throughput bar adsorptive microextraction and microliquid desorption (HT-BAμE-μLD) for the extraction and desorption of ketamine and norketamine in up to 100 urine samples simultaneously, resulting in an assay time of only 0.45 min/sample. The identification and quantification were carried out using large volume injection-gas chromatography-mass spectrometry operating in the selected ion monitoring mode (LVI-GC-MS(SIM)). Several parameters that could influencing HT-BAµE were assayed and optimized in order to maximize the recovery yields of ketamine and norketamine from aqueous media. These included sorbent selectivity, desorption solvent and time, as well as shaking rate, microextraction time, matrix pH, ionic strength and polarity. Under optimized experimental conditions, suitable sensitivity (1.0 μg L), accuracy (85.5-112.1%), precision (≤15%) and recovery yields (84.9-105.0%) were achieved. Compared to existing methods, the herein described analytical cycle is much faster, environmentally friendly and cost-effective for the quantification of ketamine and norketamine in urine samples. To our knowledge, this is the first work that employs a high throughput based microextraction approach for the simultaneous extraction and subsequent desorption of ketamine and norketamine in up to 100 urine samples simultaneously.
我们开发、优化并验证了一个快速分析周期，该周期使用高通量棒吸附微萃取和微液解吸（HT-BAμE-μLD）同时提取和解吸多达 100 个尿液样本中的氯胺酮和去甲氯胺酮，分析时间仅为 0.45 分钟/样本。采用大体积进样-气相色谱-质谱联用（LVI-GC-MS（SIM））进行鉴定和定量。测定并优化了可能影响 HT-BAµE 的几个参数，以最大限度地提高氯胺酮和去甲氯胺酮从水介质中的回收率。这些参数包括吸附剂选择性、解吸溶剂和时间，以及振摇速率、微萃取时间、基质 pH 值、离子强度和极性。在优化的实验条件下，实现了适当的灵敏度（1.0 μg L）、准确性（85.5-112.1%）、精密度（≤15%）和回收率（84.9-105.0%）。与现有方法相比，该分析周期速度更快、更环保、更具成本效益，可用于同时提取和随后解吸多达 100 个尿液样本中的氯胺酮和去甲氯胺酮。据我们所知，这是首次采用高通量微萃取方法同时提取和随后解吸多达 100 个尿液样本中的氯胺酮和去甲氯胺酮。
