固相微萃取-HPLC测定生物样品中异丙酚含量

Content Determination of Propofol in Biological Samples by Solid Phase Microextraction-HPLC

关键词:  异丙酚  固相微萃取  高效液相色谱法  生物样品

Key words:  propofol  solid phase microextraction  HPLC  biological samples

摘要:

目的 采用固相微萃取（solid phase microextraction，SPME）-HPLC联用技术测定生物样品中异丙酚的含量。方法 采用Oasis HLB固相微萃取小柱对样品进行前处理，Shim-pack VP-ODS色谱柱（250 mm×4.6 mm，5 μm），乙腈-水（1%三氟乙酸调pH值至4.00）（70：30）为流动相，流速1.0 mL·min^-1，激发波长276 nm，发射波长301 nm，柱温40℃。结果 异丙酚和卡马西平分离度良好。异丙酚在1.2~21.0 mg·L^-1内线性关系良好（r=0.999 7），平均方法回收率为98%~104%，RSD<5%；日内、日间精密度RSD均<5%。结论 该方法简便、专属性好，能有效消除部分内源性物质的干扰，适用于异丙酚的血药浓度监测和临床药动学研究。

Abstract:

OBJECTIVE To establish a method for the content determination of propofol in biological samples by solid phase microextraction(SPME)-HPLC. METHODS Samples were pretreated by Oasis HLB-SPME column and analyzed by HPLC consisting of a Shim-pack VP-ODS colum (250 mm×4.6 mm, 5 μm), and using a mixture solution of acetonitrile-water (adjusting the pH to 4.00 with 1% trifluoroacetic acid) (70:30) as the mobile phase. The flow rate was 1.0 mL·min^-1, the excitation wavelength was 276 nm, the emission wavelength was 301 nm, and the column temperature was 40℃. RESULTS The separation of propofol and carbamazepine was good. The method showed a good linearity in the range of 1.2-21.0 mg·L^-1(r=0.999 7). The methodological recoveries were all between 98% and 104%, the RSD was <5%. Intraday and interday precision were <5%. CONCLUSION This method is simple and specific, and can effectively eliminate the interference of certain endogenous substances. It is suitable for the therapeutic drug monitoring of propofol in clinic and pharmacokinetic studies.