Journal of Chromatography B ( IF 3 ) Pub Date : 2018-03-08 , DOI: 10.1016/j.jchromb.2018.03.011 Paweł Szpot , Grzegorz Buszewicz , Tomasz Jurek , Grzegorz Teresiński
This paper presents a rapid, sensitive and precise method for the determination of metaldehyde in human blood, using ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry and high-performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry. Separation was performed with a Poroshell 120 EC-C18 column; 2.7 μm atrazine‑d5 (IS) and 200 mg NaCl were added to the blood sample. Proteins in human blood were precipitated using acetonitrile; the supernatant was then analyzed with the UHPLC-Q-TOF-MS or HPLC-QqQ-MS/MS system. The results of selectivity, linearity, accuracy, precision, limits of quantification, recovery, and matrix effects were sufficient to enable the measurement of metaldehyde in human blood samples. In addition, we proposed a fragmentation pathway involving ammonium adduct fragment ions for metaldehyde.
中文翻译:
涉及加合物铵碎片离子的碎片模式:HPLC-QqQ-MS / MS和UHPLC-Q-TOF-MS测定人血中甲醛的比较
本文提供了一种快速,灵敏,精确的测定人血中乙醛的方法,该方法采用了超高效液相色谱与四极杆飞行时间串联质谱联用,以及高效液相色谱与三重四极杆串联质谱联用。用Poroshell 120 EC-C18色谱柱进行分离。将2.7μm阿特拉津-d5(IS)和200 mg NaCl添加到血液样本中。用乙腈沉淀人血中的蛋白质;然后用UHPLC-Q-TOF-MS或HPLC-QqQ-MS / MS系统分析上清液。选择性,线性,准确度,精密度,定量限,回收率和基质效应的结果足以进行人血样品中甲醛的测定。此外,