El-Beqqali Aziza, Abdel-Rehim Mohamed
Department of Chemistry, Karlstad University, Karlstad, Sweden.
J Sep Sci. 2007 Oct;30(15):2501-5. doi: 10.1002/jssc.200700067.
A method for the simultaneous analysis of methadone in urine samples by microextraction in a packed syringe online with GC-MS (MEPS-GC-MS) is described. The new method reduced the sample handling and the detection limit by two- to seven-fold compared to published methods. Using a quantitation method based on the calculation of analyte concentration by comparison to an internal standard, we were able to measure methadone levels consistent with values reported for healthy individuals. The intra-assay precisions (RSD) of the method using quality control (QC) samples at three different concentration levels were about 11-14% (n = 6). The interassay precisions (RSD) were 11-15% for methadone in urine samples (n = 18). The accuracy varied from 89 to 109% for intra-assay (n = 6), and 97 to 107% for inter-assay (n = 18). The regression correlation coefficients (r(2)) were over 0.99 in all experiments.
描述了一种通过填充注射器在线微萃取结合气相色谱-质谱联用(MEPS-GC-MS)同时分析尿液样本中美沙酮的方法。与已发表的方法相比,新方法将样品处理量和检测限降低了两到七倍。使用基于与内标比较计算分析物浓度的定量方法,我们能够测量出与健康个体报告值一致的美沙酮水平。使用三种不同浓度水平的质量控制(QC)样品,该方法的批内精密度(RSD)约为11-14%(n = 6)。尿液样本中美沙酮的批间精密度(RSD)为11-15%(n = 18)。批内准确度在89%至109%之间(n = 6),批间准确度在97%至107%之间(n = 18)。所有实验中的回归相关系数(r²)均超过0.99。