Journal of Chromatography B ( IF 2.8 ) Pub Date : 2008-12-25 , DOI: 10.1016/j.jchromb.2008.12.036 W. Xie , W.M. Mullett , C.M. Miller-Stein , J. Pawliszyn
Studies using in-tip solid phase microextraction (in-tip SPME) in a 96-well plate format are conducted to investigate the feasibility of SPME automation. The sample preparation process, including extraction and desorption, was fully automated and coupled with currently commercially available automated liquid handling systems. Several process parameters including extraction time and speed, and desorption time were investigated. An LC–MS/MS method has been developed and validated to determine the levels of a drug compound (MK-0533) in human plasma that demonstrates the suitability of this new approach. The developed method has a lower limit of quantitation (LLOQ) of 5 ng/mL when 0.25 mL of human plasma is processed and is validated in the concentration range of 5–2000 ng/mL. The successful application of the assay in clinical sample analysis indicates that in-tip SPME can be easily automated and has great potential to be used for high throughput quantitative determination of drugs in pharmaceutical industry.
中文翻译:
液相色谱-串联质谱检测法以96孔格式进行尖端固相微萃取自动化,以测定人血浆中的模型药物
进行了以96孔板形式使用尖端固相微萃取(尖端SPME)的研究,以研究SPME自动化的可行性。样品制备过程(包括提取和解吸)是完全自动化的,并与当前市售的自动化液体处理系统结合在一起。研究了几个工艺参数,包括萃取时间和速度以及脱附时间。已经开发出一种LC-MS / MS方法,并经过验证可以确定人血浆中药物化合物(MK-0533)的水平,这证明了这种新方法的适用性。当处理0.25 mL人体血浆时,开发的方法的定量下限(LLOQ)为5 ng / mL,并在5–2000 ng / mL的浓度范围内得到验证。