毛細管膠束電動色譜法分離測定中藥半枝蓮中的7種有效成分

米 璇, 朱若華

(首都師范大學化學系,北京100048)

毛細管膠束電動色譜法分離測定中藥半枝蓮中的7種有效成分

米 璇, 朱若華＊

(首都師范大學化學系,北京100048)

建立了毛細管膠束電動色譜同時分析檢測中藥半枝蓮藥材及其膏劑中黃芩素、柚皮素、漢黃芩素、野黃芩苷、芹菜素、木犀草素和原兒茶酸7種有效成分的方法。半枝蓮樣品中7種有效成分經甲醇超聲提取。實驗考察了運行緩沖溶液的pH值和濃度、添加劑、檢測波長、分離電壓和進樣時間等重要參數對目標物分離的影響。得到的優化條件為:運行緩沖液50mmol/L硼砂-0.20mol/L硼酸溶液(pH8.4),含8.5mmol/L十二烷基硫酸鈉(SDS),分離電壓25kV,檢測波長260nm和335nm。在此條件下,7種組分于12m in內達到基線分離。各組分在8×10-6～3.2×10-4mol/L范圍內呈良好的線性關系,相關系數(r2)為0.996 5～0.999 9;檢出限為7.0×10-8～2.0×10-6mol/L;回收率均大于85%。該方法提取簡便、準確可靠、重復性好、靈敏度高,可以用于中藥半枝蓮中7種有效成分的定量檢測。

膠束電動色譜;半枝蓮;有效成分;中草藥

Abstract:A method of capillary micellar electrokinetic chromatography with a diode array detector was developed for the simultaneous determ ination of7active ingredients(baicalein,naringenin,wogonin,scutellarin,apigenin,luteolin,and protocatechuic acid)in Scutella riabarbata D.D on and its ointment.The7ingredients in samples were extracted with m ethanol in an ultrasonic bath.The important factors,such as pH,running buffer concentration,additive,detection wavelength,separation voltage and injection time,were optimized.Under the optimum conditions,the7 analytes were separated within12m in at a separation voltage of25kV in a50 mmol/L borate-0.20mol/L boric acid buffer(pH8.4)containing8.5mmol/L sodium dodecyl sulfate(SDS).The detection was carried out at260nm and335nm.N otably,the linearity ranged from8×10-6to3.2×10-4mol/L with the correlation coefficients(r2)at the range of 0.996 5-0.999 9.The detection limits(S/N=3)ranged from7.0×10-8mol/L to2.0×10-6mol/L for all the7analytes.The recoveries of the7active ingredients were all over85%.This method is of good sensitivity,simple preparation,good rep roducibility and reliability.It was successfully applied to the analysis of the7active ingredients in Scutella riabarbata D.D on and its ointment.

Key words:micellar electrokinetic chromatography(M EKC);Scutella riabarbata D.D on;active ingredients;Chinese medicinal herb

半枝蓮為唇形科黃芩屬植物Scu tella ria ba rba ta D.D on的干燥全草[1],別名通經草、紫連草、并頭草、牙刷草、小韓信草等。其性辛、苦、寒,入肺、肝、腎,具有清熱解毒、化淤利尿的功效,用于治療疔瘡腫毒、咽喉腫痛、毒蛇咬傷、跌撲腫痛、水腫、黃疸等[2]。半枝蓮作為臨床常用中藥,廣泛應用于抗炎、抗癌等方面,是近年來國內外抗腫瘤中藥的研究熱點之一。但是對于其藥理活性的物質基礎,特別是關于抗腫瘤作用的有效成分及其機制的研究并不深入。這些原因使得半枝蓮多以草藥煎劑出現,并未開發出療效明確的單體成分劑型?！?br>