Szpot Paweł, Buszewicz Grzegorz, Jurek Tomasz, Teresiński Grzegorz
Department of Forensic Medicine, Wrocław Medical University, ul. Jana Mikulicza-Radeckiego 4, 50-345 Wrocław, Poland.
Department of Forensic Medicine, Medical University of Lublin, ul. Jaczewskiego 8b, 20-090 Lublin, Poland.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 May 15;1085:104-109. doi: 10.1016/j.jchromb.2018.03.011. Epub 2018 Mar 8.
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.
本文介绍了一种快速、灵敏且精确的测定人血中聚乙醛的方法，该方法采用超高效液相色谱-四极杆飞行时间串联质谱联用以及高效液相色谱-三重四极杆串联质谱联用技术。使用Poroshell 120 EC-C18柱（2.7μm）进行分离；向血样中加入2.7μm的莠去津-d5（内标）和200mg氯化钠。采用乙腈沉淀人血中的蛋白质；然后将上清液用超高效液相色谱-四极杆飞行时间质谱仪或高效液相色谱-三重四极杆串联质谱仪系统进行分析。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用于测定人血样中的聚乙醛。此外，我们提出了一种涉及聚乙醛铵加合物碎片离子的裂解途径。
