【摘要】 建立了同时测定复方杏香兔耳风胶囊中原儿茶酸、原儿茶醛、绿原酸、野黄芩苷、异绿原酸C、黄芩苷、木犀草素、芹菜素、白术内酯III和白术内酯I等10种有效成分含量的超高效液相色谱-串联质谱(UPLC-MS/MS)双内标分析方法。以咖啡酸和淫羊藿苷为内标(IS),在ZORBAX RRHD Eclipse Plus C18色谱柱上,以甲醇和含0.3%甲酸的水为流动相进行梯度洗脱分离,流速为0.3 mL/min。在电喷雾电离(ESI)正、负离子切换模式下,采用多重反应监测模式进行检测。结果表明,原儿茶酸、原儿茶醛、绿原酸、野黄芩苷、异绿原酸C、黄芩苷、木犀草素、芹菜素、白术内酯III、白术内酯I的线性范围分别为0.003 00~24.0 mg/L、0.017 0~2.00 mg/L、0.015 0~30.0 mg/L、0.004 00~30.0 mg/L、0.010 5~24.0 mg/L、0.003 00~30.0 mg/L、0.003 00~5.00 mg/L、0.006 00~5.00 mg/L、0.001 50~4.00 mg/L、0.000 600~0.900 mg/L;检出限分别为1.0、11、5.0、1.5、3.5、1.0、1.0、2.0、0.50、0.20μg/L。10种成分的加样回收率为92.5%~106%,相对标准偏差均不大于3.2%。该方法快速简便、灵敏度高、重复性好,已成功用于实际样品的分析。更多还原

【Abstract】 Usin g caffeic acid and icariin as internal standards,a method for the simultaneous determination of protocatechuic acid,p rotocatechuic aldehyde,chloro g enic acid,scutellarin,isochlorogenic acid C,baicalin,luteolin,a p i g enin,atract y lenolide III and atractylenolide I in Fufangxingxian g tu’erfen g ca p sules were established by ultra performance liquid chromatography with tandem mass spectrometry(UPLC-MS/MS).The separation was performed on a ZORBAX RRHD Eclipse Plus C18column(50 mm×2.1 mm,1.8μm)b y usin g water containing 0.3% formic acid and methanol as mobile phases with the gradient elution at a flow rate of 0.3 mL/min.The analytes were detected by a tandem mass spectrometer in the multiple reaction monitoring(MRM)mode via the switching of positive electrospray ionization(ESI+)and negative electrospray ionization(ESI-).Under optimum conditions,the calibration curves were linear in the range of 0.003 00-24.0 mg/L for protocatechuic acid,0.017 0-2.00 mg/L for protocatechuic aldehyde,0.015 0-30.0 mg/L for chlorogenic acid,0.004 00-30.0 mg/L for scutellarin,0.010 5-24.0 mg/L for isochloro g enic acid C,0.003 00-30.0 mg/L for baicalin,0.003 00-5.0 mg/L for luteolin,0.006 00-1.50 mg/L for apigenin,0.001 50-4.00 mg/L for atractylenolide III,and 0.000 600-0.900 mg/L for atractylenolide I with the detection limits of 1.0,11,5.0,1.5,3.5,1.0,1.0,2.0,0.50,0.20μg/L,res p ectivel y.The average recoveries of the ten effective components were between92.5% and 106% with all relative standard deviations not more than3.2%.The developed method was rapid,sim p le,accurate,re p roducible,and suitable for the quality control of the Fufangxin g xian g tu’erfen g ca p sules.更多还原