Abstract The quantitative determination of drugs in urine by high performance liquid chromatography electrospray-ionization mass spectrometry (HPLC-ESI-MS) is challenging due to complex matrix interferences and the relatively low concentrations of analytes in urine. In this study, porous graphitic carbon (PGC) was investigated as solid phase extraction (SPE) sorbent before HPLC-ESI-MS determination of three 5-hydroxytryptamine (3) (5-HT3) receptor antagonists from human urine. The factors affecting extraction of the target antagonists were investigated and optimized systematically by using single-factor tests. The optimized SPE procedure was developed for the simultaneous extraction and sample pretreatment of tropisetron, ondansetron, and granisetron in urine by HPLC-ESI-MS/MS. Using the optimized conditions, the matrix effects were reduced by the PGC-based SPE clean-up procedure, with acceptable matrix effects for tropisetron, ondansetron, and granisetron from 96.53% to 98.42%, 93.19% to 94.36%, and 94.48% to 95.60%, respectively. The reported method significantly removes matrix interferences from the urine samples and exhibited satisfactory recovery and process efficiency for the determination of tropisetron, ondansetron, and granisetron. The established pretreatment method provides a promising strategy for the removal of interferences from hydrophilic basic drugs in biological fluids.

中文翻译：

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多孔石墨碳 (PGC) 固相萃取 (SPE) 结合高效液相色谱-串联质谱 (HPLC-MS/MS) 测定人尿液中的 5-HT3 受体拮抗剂

摘要 由于复杂的基质干扰和尿液中分析物的相对低浓度，通过高效液相色谱电喷雾电离质谱 (HPLC-ESI-MS) 定量测定尿液中的药物具有挑战性。在本研究中，在 HPLC-ESI-MS 测定人尿中的三种 5-羟色胺 (3) (5-HT3) 受体拮抗剂之前，研究了多孔石墨碳 (PGC) 作为固相萃取 (SPE) 吸附剂。采用单因素检验对影响靶拮抗剂提取的因素进行系统研究和优化。开发了优化的 SPE 程序，用于通过 HPLC-ESI-MS/MS 同时提取和样品预处理尿液中的托烷司琼、昂丹司琼和格拉司琼。使用优化条件，基于 PGC 的 SPE 净化程序降低了基质效应，托烷司琼、昂丹司琼和格拉司琼的可接受基质效应分别从 96.53% 到 98.42%、93.19% 到 94.36% 和 94.48% 到 95.60%。所报告的方法显着消除了尿液样品中的基质干扰，并且在测定托烷司琼、昂丹司琼和格拉司琼时表现出令人满意的回收率和工艺效率。已建立的预处理方法为去除生物体液中亲水性碱性药物的干扰提供了一种有前景的策略。所报告的方法显着消除了尿液样品中的基质干扰，并且在测定托烷司琼、昂丹司琼和格拉司琼时表现出令人满意的回收率和工艺效率。已建立的预处理方法为去除生物体液中亲水性碱性药物的干扰提供了一种有前景的策略。所报告的方法显着消除了尿液样品中的基质干扰，并且在测定托烷司琼、昂丹司琼和格拉司琼时表现出令人满意的回收率和工艺效率。已建立的预处理方法为去除生物体液中亲水性碱性药物的干扰提供了一种有前景的策略。