Department of Chemistry, University of Waterloo, 200 University Avenue West, Waterloo, Ontario, N2L 3G1, Canada.
Department of Chemistry, University of Waterloo, 200 University Avenue West, Waterloo, Ontario, N2L 3G1, Canada.
Talanta. 2021 Sep 1;232:122438. doi: 10.1016/j.talanta.2021.122438. Epub 2021 Apr 22.
UPLC-MS/MS methods are the gold standard for routine, high-throughput measurements of biogenic monoamines for the diagnosis of catecholamine-producing tumors. However, this cannot be achieved without employing efficient sample pretreatment methods. Therefore, two pretreatment methods, thin-film solid phase microextraction (TF-SPME) and packed fibers solid phase extraction (PFSPE), were developed and evaluated for the analysis of biogenic monoamines and their metabolites in urine. A hydrophilic-lipophilic balance (HLB) coating was chosen for the thin-film blade format SPME method and compared with a Polycrown ether (PCE) composite nanofiber used as an adsorbent for the PFSPE method. Under optimal conditions, the absolute extraction recovery and relative matrix effect of the newly developed TF-SPME method were determined to be 35.7-74.8% and 0.47-3.63%, respectively. The linearity was 0.25-500 ng mL for norepinephrine, epinephrine, dopamine, normetanephrine 3-methoxytyramine, serotonin, histamine, and 0.1-500 ng mL for metanephrine. The intra-and inter-assay coefficients of variation were 0.7-8.7%, and the respective accuracies were calculated to be 90.8-104.7% and 89.5-104.5% for TF-SPME. Compared with the PFSPE method, the TF-SPME method had a higher extraction efficiency, lower matrix effects and a wider linear range for eight target substances, which ensured higher accuracy of simultaneous detection of all compounds of interest. Therefore, the proposed TF-SPME method can be employed for the high throughput screening for neuroendocrine tumors in a routine clinical setting and other relative research by simultaneous quantitation of urine eight biological monoamines in a single run.
UPLC-MS/MS 方法是常规高通量测量生物单胺用于诊断儿茶酚胺产生肿瘤的金标准。然而，如果不采用有效的样品预处理方法，这是无法实现的。因此，开发并评价了两种预处理方法，即薄膜固相微萃取（TF-SPME）和填充纤维固相萃取（PFSPE），用于分析尿液中的生物单胺及其代谢物。亲水-亲脂平衡（HLB）涂层被选为薄膜刀片格式 SPME 方法的涂层，并与用作 PFSPE 方法吸附剂的聚冠醚（PCE）复合纳米纤维进行了比较。在最佳条件下，新开发的 TF-SPME 方法的绝对萃取回收率和相对基质效应分别确定为 35.7-74.8%和 0.47-3.63%。对于去甲肾上腺素、肾上腺素、多巴胺、去甲变肾上腺素 3-甲氧基酪胺、血清素、组胺和 0.1-500ng mL 的线性范围为 0.25-500ng mL，对于甲氧基肾上腺素的线性范围为 0.1-500ng mL。TF-SPME 的日内和日间变异系数分别为 0.7-8.7%，各自的准确度计算为 90.8-104.7%和 89.5-104.5%。与 PFSPE 方法相比，TF-SPME 方法具有更高的萃取效率、更低的基质效应和更宽的 8 种目标物的线性范围，这确保了对所有感兴趣化合物的同时检测具有更高的准确性。因此，该提议的 TF-SPME 方法可用于常规临床环境中的神经内分泌肿瘤的高通量筛选，以及通过单次运行同时定量分析尿液中的 8 种生物单胺进行其他相关研究。
