活性炭固相萃取/胶束电动色谱联用技术用于雷公藤3种有效成分的测定  

Determination of Three Active Components in Tripterygium Wilfordii Hook F. by Activated Carbon Solid Phase Extraction Combined with Micellar Electrokinetic Capillary Chromatography

作　　者：蒋银燕[1] 郭丽娟[1] 崔小莹[1] 王翠琼 胡小建[1] 李建明[2] 

机构地区：[1]长沙医学院基础医学院,湖南长沙410219 [2]中南大学湘雅医学院,湖南长沙410013

出　　处：《分析测试学报》2015年第2期189-193,共5页Journal of Instrumental Analysis

基　　金：湖南省科技厅科技计划项目(2014SK3025);湖南省教育厅科学研究项目(12C0489;12B018;13C1125);长沙市科技计划项目(K1207042-31)

摘　　要：建立了活性炭固相萃取/胶束电动色谱法同时测定中药雷公藤中的雷公藤甲素、雷公藤内酯酮和雷酚内酯的方法。优化了萃取p H值、乙醇洗脱体积、电泳运行缓冲溶液p H值与浓度、胶束SDS的浓度及进样时间、电压等条件。进行电泳分离之前,分析物用活性炭进行吸附后用2.0 m L乙醇洗脱。在214 nm波长处,分离电压20 k V,20 mmol/L硼酸-10 mmol/L硼砂（p H 8.0）-20 mmol/L SDS运行缓冲溶液条件下,3种成分在8 min内得到完全分离,雷公藤甲素、雷公藤内酯酮在4.0×10^-5-4.0×10^-3mol/L,雷酚内酯在4.0×10^-5-1.0×10^-3mol/L浓度范围内线性关系良好,其回收率为81.0%-102.9%,方法的检出限分别为1.42×10^-6,7.90×10^-7,2.96×10^-7mol/L,相对标准偏差（RSD）分别为3.2%,5.4%,3.5%。所建立的方法简单、快速、准确,成功用于雷公藤片样品的测定。A method has been developed for simultaneous determination of triptolide,triptonide and triptophenolide in traditional Chinese herb Tripterygium wilfordii Hook F. by micellar electrokinetic capillary chromatography（ MEKC） combined with activated carbon solid phase extraction. Effects of some important factors,such as p H value of extraction,eluant volume of ethanol,p H value and concentration of running buffer,concentration of sodium dodecyl sulfate（ SDS）,separation voltage and injection time were investigated. The analytes were extracted with activated carbon in phosphate buffer solution（ p H 6. 5）,then eluted with 2. 0 m L ethanol before separated by MEKC. At 214 nm wavelength,the detection analytes could be well separated within 8 min at separation voltage of 20 k V in 20 mmol / L boric acid- 10 mmol / L borax（ p H 8. 0）- 20 mmol / L SDS. Under the optimized conditions,the calibration curves were linear in the range of 4. 0 × 10^- 5- 4. 0 × 10^- 3mol / L for triptolide and the triptonide,and 4. 0 × 10^- 5- 1. 0 × 10^- 3mol / L for triptophenolide. The detection limits of triptolide,triptonide and triptophenolide were 1. 42 × 10^- 6,7. 90 × 10^- 7,2. 96 × 10^- 7mol / L,respectively,and the relative standard deviations（ RSDs,n = 6） for peak areas were 3. 2%,5. 4%,3. 5%,respectively. The proposed method had the advatages of simplicity,rapidness,low sample consumption and accuracy, and was successfully applied in the determination of the analytes in Tripterygium wilfordii tablet with recoveroes of 81. 0%- 102. 9%.

关 键 词：雷公藤甲素 雷公藤内酯酮 雷酚内酯 固相萃取 胶束电动色谱 

分 类 号：O657.7[理学—分析化学] TQ460.72[理学—化学]