A simultaneous extraction/derivatization strategy coupled with liquid chromatography–tandem mass spectrometry for the determination of free catecholamines in biological fluids
【作者】Di Chen, Jing-Xian Zhang, Wei-Qi Cui, Jun-Wei Zhang, De-Qiao Wu, Xin-Rui Yu, Yan-Bo Luo, Xing-Yi Jiang, Feng-Peng Zhu, Dilshad Hussain, Xia Xu*
【期刊名】Journal of Chromatography A
【影响因子】2021年: 4.759
【作者单位】School of Pharmaceutical Sciences, Zhengzhou University, 100 Kexue Avenue, Zhengzhou 450001, PR China
【年，卷(期)：页码】2021, 1654: 462474
【关键词】Catecholamines, Simultaneous extraction/derivatization pretreatment method, UPLC-MS/MS, Pheochromocytoma
【摘要】The current study presents a convenient, rapid and effective simultaneous extraction/derivatization (SEDP) strategy for effective pretreatment of catecholamines (CAs). Commercial zirconium oxide (ZrO2) nanoparticles were employed for the selective capturing of cis-diol containing CAs to remove the biological interferences and phenyl isothiocyanate (PITC) was used for derivatization to improve the ionization and to improve the chromatographic separation. The extraction and derivatization procedures were integrated into one step to simplify the sample pretreatment. Excessive derivatization reagents were removed as well, reducing the degree of contaminations in mass spectrometry. The factors affecting the SEDP process were optimized and the results showed that the detection sensitivity and chromatographic separation of CAs greatly improved compared with underivatized CAs, during LC-MS/MS analysis. Combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), quantifying the concentration of norepinephrine (NE), epinephrine (E) and dopamine (DA) in biological fluids was validated in ranges of 1-200.0 ng/mL with a satisfactory correlation coefficient (R2 > 0.997). The obtained recoveries were in the range of 91.0-109.5% with RSDs less than 9.4%. Finally, significant changes in CAs levels in urine samples of healthy people and pheochromocytoma patients were detected. The developed method offers comparative advantages in terms of sensitivity, specificity and selectivity.
【全文链接】https://www.sciencedirect.com/science/article/abs/pii/S0021967321005987
