The State Laboratory, Backweston Laboratory Complex, Young's Cross, Celbridge, Co., Kildare, Ireland.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Feb 1;879(3-4):253-9. doi: 10.1016/j.jchromb.2010.12.008. Epub 2010 Dec 21.
A rapid method has been developed to analyse CP 47, 497 in human urine. Urine samples were diluted with water:acetonitrile (90:10, v/v) and sample aliquots were analysed by triple quadrupole tandem mass spectrometry with a runtime of 5 min. Multiple reaction monitoring (MRM) as survey scan was performed. The method was validated in urine, according to an in-house validation protocol based on the criteria defined in Commission Decision 2002/657/EC. Three MRM transitions were monitored. The decision limit (CCα) was 0.01μg mL⁻¹ and for the detection capability a (CCβ) value of 0.02 μg mL⁻¹ was obtained. The measurement uncertainty of the method was 21%. Fortifying human urine samples (n=18) in three separate assays, show the accuracy of the method to be between 95 and 96%. The precision of the method, expressed as RSD values for the within-lab reproducibility at the three levels of fortification (0.1, 0.15 and 0.2 μg mL⁻¹) was less than 10% respectively. The method proved to be simple, robust and time efficient. To the best of our knowledge there are no LC-MS methods for the determination of CP 47, 497 with validation data in urine.
已经开发出一种快速分析人尿中 CP 47,497 的方法。尿样用水：乙腈（90:10，v/v）稀释，用三重四极杆串联质谱仪在 5 分钟的运行时间内进行分析。采用多重反应监测（MRM）作为总扫描进行分析。该方法按照基于委员会决定 2002/657/EC 中定义的标准的内部验证方案在尿中进行了验证。监测了三个 MRM 跃迁。决策限（CCα）为 0.01μg mL⁻¹，检测能力（CCβ）值为 0.02μg mL⁻¹。该方法的测量不确定度为 21%。在三个单独的测定中对人尿样（n=18）进行加标，表明该方法的准确度在 95%至 96%之间。该方法的精密度（表示为三个加标水平（0.1、0.15 和 0.2μg mL⁻¹）的实验室内重现性的 RSD 值）分别小于 10%。该方法简单、稳健且高效。据我们所知，目前尚无 LC-MS 方法可用于验证尿中 CP 47,497 的含量。
