Yilmaz Bilal, Erdem Ali Fuat
Department of Analytical Chemistry, Faculty of Pharmacy, Ataturk University, Erzurum 25240, Turkey
Department of Anesthesiology and Reanimation, Faculty of Medicine, Sakarya University, Sakarya 54187, Turkey.
J Chromatogr Sci. 2015 Aug;53(7):1037-43. doi: 10.1093/chromsci/bmu214. Epub 2015 Jan 22.
A sensitive and efficient method was developed for determination of tramadol and its metabolite (O-desmethyltramadol) in human urine by gas chromatography-mass spectrometry. Tramadol, O-desmethyltramadol and medazepam (internal standard) were extracted from human urine with a mixture of ethylacetate and diethylether mixture (1 : 1, v/v) at basic pH with liquid-liquid extraction. The calibration curves were linear (r = 0.99) over tramadol and O-desmethyltramadol concentrations ranging from 10 to 200 ng/mL and 7.5 to 300 ng/mL, respectively. The method had an accuracy of >95% and intra- and interday precision (relative standard deviation %) of ≤4.93 and ≤4.62% for tramadol and O-desmethyltramadol, respectively. The extraction recoveries were found to be 94.1 ± 2.91 and 96.3 ± 3.46% for tramadol and O-desmethyltramadol, respectively. The limit of quantification using 0.5 mL human urine was 10 ng/mL for tramadol and 7.5 ng/mL for O-desmethyltramadol. After oral administration of 100 mg of tramadol hydrochloride to a patient, the urinary excretion was monitored during 24 h. About 15% of the dose was excreted as unchanged tramadol.
建立了一种灵敏、高效的气相色谱-质谱法测定人尿中曲马多及其代谢物（O-去甲基曲马多）的方法。采用液-液萃取法，在碱性pH条件下，用乙酸乙酯和乙醚混合液（1:1，v/v）从人尿中提取曲马多、O-去甲基曲马多和地西泮（内标）。曲马多和O-去甲基曲马多浓度分别在10至200 ng/mL和7.5至300 ng/mL范围内时，校准曲线呈线性（r = 0.99）。该方法的准确度>95%，曲马多和O-去甲基曲马多的日内和日间精密度（相对标准偏差%）分别≤4.93%和≤4.62%。曲马多和O-去甲基曲马多的萃取回收率分别为94.1±2.91%和96.3±3.46%。使用0.5 mL人尿时，曲马多的定量限为10 ng/mL，O-去甲基曲马多的定量限为7.5 ng/mL。给一名患者口服100 mg盐酸曲马多后，监测24小时内的尿排泄情况。约15%的剂量以未变化的曲马多形式排泄。
