【摘要】 目的建立黄芪药材高效液相-质谱检测器(HPLC-MS)总离子流色谱指纹图谱的评价方法。方法确定实验条件并进行方法学考察,色谱条件:agilent zorbax SB Cl8色谱柱(4.6 mm×250 mm,5μm);流动相:A相为乙腈,B相为水,梯度洗脱;流速:1.0 mL.min-1,柱后分流;柱温:室温;进样量:10μL。质谱条件:大气压电离-电喷雾电离(API-ESI)离子源;负离子检测模式;扫描范围:m/z200~1 000;干燥气(N2)流速:9.0 L.min-1;雾化气压力:206.7 kPa;干燥气温度:350℃;裂解电压:110 V;毛细管电压:3 500 V。黄芪药材以甲醇超声提取30 min。采用国家药典委员会的《中药色谱指纹图谱相似度评价系统A版》软件进行指纹图谱分析。结果黄芪药材HPLC-MS总离子流色谱指纹图谱具有较好的稳定性、精密度和重复性,相对保留时间和相对峰面积的RSD均小于4.5%,标定13个共有峰,相似度计算结果均大于0.94。结论本研究将有助于加强黄芪药材的质量控制,能够有效的区分黄芪药材同其他相关样品。更多还原

【Abstract】 OBJECTIVE To establish an evaluation method of Radix astragali by HPLC-MS total ionic chromatographic fingerprints.METHODS The conditions of experiment were confirmed and the validation of the method was also tested.The separation was performed on an agilent zorbax SB C_l8 column（4.6 mm×250 mm,5 μm） with a gradient elution.The mobile phase consisted of A（ACN） and B(H₂O).The gradient elution,flow speed was 1.0 mL·min^-1.The temperature of column was room temperature,inject volume was 10 μL.The atmosphere pressure ionization-electrospray was used with negative scan mode.The flow rate drying gas(N₂) was 9.0 L·min^-1,nebulizer pressure was 206.7 kPa,drying gas temperature was 350 ℃, fragment voltage was 110 V,capillary voltage was 3 500 V.Radix astragali was extracted by ultrasonic method for 30 min with methanol.The chromatographic fingerprints were analyzed with similarity evaluation system for chromatographic fingerprint of TCM（A edition） that issued by committee of national pharmacopoeia.RESULTS HPLC-MS total ionic chromatographic fingerprints of Radix astragali showed good stability,precision and reproducibility.The RSDs of relative retention of times and peak areas were less than 4.5%,13 common peaks were demarcated and the results of similarity calculation were more than 0.94.CONCLUSION The study is helpful for the quality control of Radix astragali,also can effectively distinguish Radix astragali from other samples.更多还原