Thienpont L M, Verhaeghe P G, De Leenheer A P
Laboratoria voor Medische Biochemie, Klinische Analyse, Rijksuniversiteit Gent, Belgium.
Biomed Environ Mass Spectrom. 1987 Nov;14(11):613-6. doi: 10.1002/bms.1200141107.
A method is described for the quantification of tulobuterol in human plasma, based upon selective extraction and high resolution capillary gas chromatography-mass spectrometry. The mass spectrometric determination is based on selected ion monitoring of two fragment ions derived from the N,O-heptafluorobutyryl derivatives of tulobuterol and its internal standard, deschlorotulobuterol. The plasma work-up procedure consists of extraction of 1.0 ml alkalinised plasma with dichloromethane, back-extraction into an acidified aqueous phase, followed by a final extraction with dichloromethane after realkalinisation. The method gave interference-free and linear results. The between-assay variability is 4.7% CV at the 3.0 micrograms l-1 plasma concentration level. The assay permitted quantitative measurements down to 170 ng tulobuterol per litre of plasma and hence provided sufficient sensitivity for quantification of plasma levels after therapeutic doses.
本文描述了一种基于选择性萃取和高分辨率毛细管气相色谱-质谱联用技术定量测定人血浆中妥洛特罗的方法。质谱测定基于对妥洛特罗及其内标去氯妥洛特罗的N,O-七氟丁酰衍生物产生的两个碎片离子进行选择离子监测。血浆处理程序包括用二氯甲烷萃取1.0 ml碱化血浆,反萃取到酸化水相中,然后在重新碱化后用二氯甲烷进行最终萃取。该方法得到无干扰的线性结果。在血浆浓度为3.0微克/升的水平下,批间变异系数为4.7%。该测定法可对低至每升血浆中170纳克的妥洛特罗进行定量测量,因此为治疗剂量后血浆水平的定量提供了足够的灵敏度。