基于HPLC及GC-MS技术的血尿胶囊融合指纹图谱  

Fusion-fingerprint of Xueniao capsules based on HPLC and GC-MS

作　　者：杨彦坤 独家能 姚静[2] 郝旭亮[2] 李媛媛[2] 王瑞明[2] 杨柳[2] 许雯雯 

机构地区：[1]山西中医药大学,太原030619 [2]山西省中医药研究院,太原030045

出　　处：《药物分析杂志》2018年第1期158-167,共10页Chinese Journal of Pharmaceutical Analysis

基　　金：山西省科技攻关项目(山西省中药现代化关键技术研究振东专项)(2014ZD0203)

摘　　要：目的:建立血尿胶囊的融合指纹图谱。方法:采用高效液相色谱(HPLC),使用C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.1%磷酸水为流动相,进行梯度洗脱,流速1.0 mL·min^(-1),检测波长280 nm,进样量10μL。采用气相色谱-质谱联用(GC-MS),使用HP-5MS色谱柱(30 m×250μm×0.25μm),载气为氦气,体积流量为1.0 mL·min^(-1),进样口温度250℃,柱温采用程序升温(初始温度45℃,保持2 min,以5℃·min^(-1)程序升温至180℃,保持10 min,后以10℃·min^(-1)程序升温至250℃,保持10 min),进样量1μL,分流比20∶1;电离方式EI,电子能量70 e V,离子源温度230℃,四极杆温度150℃,质量范围m/z 50~550。将HPLC与GC-MS的色谱数据进行归一化处理,并将数据导入国家药典委员会制定的《中药色谱指纹图谱相似度评价系统2.0版》进行指纹图谱融合。结果:在血尿胶囊融合指纹谱获得34个共有峰,HPLC指纹图谱得到22个共有峰,并指认了原儿茶酸、儿茶素、绿原酸、咖啡酸、虎杖苷、落新妇苷、黄杞苷、白藜芦醇、槲皮素9个成分,GC-MS指纹图谱鉴定了棕榈酸甲酯、棕榈酸乙酯、9,12-十八碳二烯酸甲酯、(E)-9-十八烯酸甲酯、硬脂酸甲酯、亚油酸乙酯、油酸乙酯、7,10-十八碳二烯酸甲酯、硬脂酸乙酯、11-二十烯酸甲酯、二十酸甲酯、二十二酸甲酯12个成分。结论:建立的融合指纹图谱能够全面反映血尿胶囊的整体特征,克服了单一成分含量测定及单一指纹图谱的不全面性,为复方中药制剂质量控制方法研究提供依据。Objective：To establish fusion-fingerprint of Xueniao capsules.Methods：HPLC analysis was performed on a C18 column（4.6 mm×250 mm,5 μm） with mobile phase consisting of acetonitrile-0.1% phosphoricacid with gradient elution at a flow rate of 1.0 mL·min^-1.The detection wavelength was 280 nm and the injection volume was 10 μL.GC-MS analysis was performed on an HP-5 MS column（30 m×250 μm×0.25 μm） and carrier gas was helium（He） at a flow rate of 1.0 mL·min^-1.The inlet temperature was 250 ℃.The column temperature was held at 45 ℃ for 2 min and then programmed at 5 ℃·min^-1 to 180 ℃ and held for 10 min,then at 10 ℃·min^-1 to 250 ℃ and held for 10 min.The injection volume was 1 μL and the split ratio was 20∶1.The ionization mode was EI and the electron energy was 70 e V.The ion source temperature was 230 ℃ and the quadrupole temperature was 150 ℃.The scan range was m/z 50-550.The fusion-fingerprint was originated by similarity evaluation software based on the normalized data which acquired from HPLC and GC-MS.Results：34 common peaks were found in the fusion-fingerprint of Xueniao capsules. 22 peaks were from HPLC and 9 of them were identified as protocatechuic acid,catechins,chlorogenic acid,caffeic acid,polydatin,astilbin,engeletin,resveratrol and quercetin. 12 peaks were from GC-MS and identified as hexadecanoic acid,methyl ester;hexadecanoic acid,ethyl ester;9,12-octadecadienoic acid,methyl ester;（E）-9-octadecenoic acid,methyl ester;octadecanoic acid,methyl ester;linoleic acid ethyl ester;ethyl oleate;7,10-octadecadienoic acid,methyl ester;octadecanoic acid,ethyl ester;11-eicosenoic acid,methyl ester;eicosanoic acid,methyl ester;docosanoic acid and methyl ester.Conclusion：Superior to single component quantification and single fingerprint,the proposed fusion fingerprint could reflect the comprehensive characteristics of Xueniao capsules,thus providing reference for quality control of traditional Chinese medicine preparations.

关 键 词：血尿胶囊 融合指纹图谱 原儿茶酸 儿茶素 绿原酸 咖啡酸 虎杖苷 落新妇苷 黄杞苷 白藜芦醇 槲皮素 高效液相色谱 气相色谱-质谱联用 

分 类 号：R917[医药卫生—药物分析学]