Sha Y F, Shen S, Duan G L
Department of Pharmacy, Fudan University, Shanghai 200032, PR China.
J Pharm Biomed Anal. 2005 Feb 7;37(1):143-7. doi: 10.1016/j.jpba.2004.09.050.
A simple, rapid and sensitive method for determination of tramadol in plasma samples was developed using headspace solid-phase microextraction (HS-SPME) and gas chromatography with mass spectrometry (GC-MS). The optimum conditions for the SPME procedure were: headspace extraction on a 65-microm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber; 0.5 mL of plasma modified with 0.5 mL of sodium hydroxide (0.1 M); extraction temperature of 100 degrees C, with stirring at 2000 rpm for 30 min. The calibration curve showed linearity in the range of 1-400 ng mL(-1) with regression coefficient corresponding to 0.9986 and coefficient of the variation of the points of the calibration curve lower than 10%. The detection limit for tramadol in plasma was 0.2 ng mL(-1). The proposed method was successfully applied to determination of tramadol in human plasma samples from 10 healthy volunteers after a single oral administration.
建立了一种采用顶空固相微萃取（HS-SPME）和气相色谱-质谱联用（GC-MS）测定血浆样品中曲马多的简单、快速且灵敏的方法。固相微萃取过程的最佳条件为：使用65微米聚二甲基硅氧烷/二乙烯基苯（PDMS/DVB）纤维进行顶空萃取；0.5 mL血浆用0.5 mL氢氧化钠（0.1 M）改性；萃取温度为100℃，以2000 rpm搅拌30分钟。校准曲线在1 - 400 ng mL⁻¹范围内呈线性，回归系数为0.9986，校准曲线各点的变异系数低于10%。血浆中曲马多的检测限为0.2 ng mL⁻¹。所提出的方法成功应用于10名健康志愿者单次口服给药后人体血浆样品中曲马多的测定。
