Yeh G C, Sheu M T, Yen C L, Wang Y W, Liu C H, Ho H O
Department of Pediatrics, Taipei Medical College, Taiwan, ROC.
J Chromatogr B Biomed Sci Appl. 1999 Feb 19;723(1-2):247-53. doi: 10.1016/s0378-4347(98)00514-3.
A modified high-performance chromatographic method using UV detection was developed for determination of tramadol concentration in human plasma. Plasma samples were extracted with ethyl acetate in a one-step liquid-liquid extraction (recovery 88.5+/-2.1%). Analysis of the extract was performed on a reversed-phase LiChrospher 60 RP-select B column with a particle size of 5 microm. The mobile phase consisted of 0.05 M KH2PO4 aqueous solution (pH 3.5) and acetonitrile in a ratio of 90:10 (v/v). Metoprolol was used as the internal standard and UV detection at 225 nm was employed. Accuracy of the assay in the concentration range examined was from 1.3 to 11.9% for the intra-day run and from 1.4 to 8.1% for the inter-day run. The precision of this method varied from 1.2 to 8.7%. The reproducibility of the method was determined to be from 0.8 to 7.2% over the six-day period. A limit of detection was 9 ng/ml at a signal-to-noise ratio of 3. This validated method was then applied to the determination of tramadol concentrations in healthy volunteers after oral administration of 100 mg of tramadol in capsules of Painlax and Tramal.
建立了一种使用紫外检测的改良高效色谱法，用于测定人血浆中曲马多的浓度。血浆样品通过一步液 - 液萃取用乙酸乙酯萃取（回收率88.5±2.1%）。萃取物在粒径为5微米的反相LiChrospher 60 RP - select B柱上进行分析。流动相由0.05 M KH2PO4水溶液（pH 3.5）和乙腈按90:10（v/v）的比例组成。美托洛尔用作内标，并采用225 nm处的紫外检测。在所检测的浓度范围内，该测定法的日内准确度为1.3%至11.9%，日间准确度为1.4%至8.1%。该方法的精密度在1.2%至8.7%之间变化。该方法在六天期间的重现性测定为0.8%至7.2%。在信噪比为3时，检测限为9 ng/ml。然后将这种经过验证的方法应用于在健康志愿者口服100 mg Painlax和Tramal胶囊中的曲马多后曲马多浓度的测定。
