Abuzooda Thana, Amini Ahmad, Abdel-Rehim Mohamed
Department of Analytical Chemistry, Stockholm University, 106 91 Stockholm, Sweden.
Swedish Drug Agency,751 03 Uppsala, Sweden.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Jun 15;992:86-90. doi: 10.1016/j.jchromb.2015.04.027. Epub 2015 Apr 27.
In the present work a new graphitic material (Carbon-XCOS) was used as a sorbent for microextraction by packed sorbent (MEPS). The β-blockers metoprolol and acebutolol in plasma samples were extracted and detected online using Carbon-MEPS syringe and liquid chromatography and tandem mass spectrometry (LC-MS/MS). Factors affecting the MEPS performance such as conditioning, washing and elution solutions were investigated. The validation of the bioanalytical method was performed using human plasma. The standard curve ranged from 10 to 2000nM and the lower limit of quantification (LLOQ) was set to 10nM. The method validation showed good accuracy and precision for the quality control (QC) samples at three concentration levels (30, 800 and 1600nM). The accuracy values of the QC samples were in the range of 86-108% (n=18). The precision values of intra- and inter-day for QC samples ranged from 4.4% to 14.4% (RSD) for the both studied analytes. The coefficient of determination (R(2)) values were ≥0.999 (n=3).
在本研究中，一种新型石墨材料（Carbon-XCOS）被用作填充吸附剂微萃取（MEPS）的吸附剂。使用Carbon-MEPS注射器以及液相色谱-串联质谱法（LC-MS/MS）对血浆样本中的β受体阻滞剂美托洛尔和醋丁洛尔进行在线萃取和检测。研究了影响MEPS性能的因素，如调节、洗涤和洗脱溶液。使用人血浆对生物分析方法进行验证。标准曲线范围为10至2000nM，定量下限（LLOQ）设定为10nM。方法验证表明，在三个浓度水平（30、800和1600nM）下，质量控制（QC）样品具有良好的准确度和精密度。QC样品的准确度值在86-108%范围内（n = 18）。对于两种研究的分析物，QC样品日内和日间的精密度值范围为4.4%至14.4%（相对标准偏差）。决定系数（R²）值≥0.999（n = 3）。
