[关键词]
[摘要]
目的 采用HPLC-ELSD法建立知母的指纹图谱,全面综合反映和控制知母整体质量。方法 Thermo色谱柱C8(250mm×4.6 mm,5 μm),流动相为乙腈(A)-0.2%冰醋酸水溶液(B)梯度洗脱:0~5 min,5%~7%A;5~15 min,7%~15%A;15~36 min,15%~22%A;36~43 min,22%~35%A;43~51 min,35%~50%A;51~60 min,100%A;柱温25℃,体积流量1 mL/min,ELSD检测器雾化器(空气)体积流量2.6 L/min,漂移管温度100℃,进样量20 μL。结果 在60 min内获得了较好分离效果的特征图谱,确定12个主要特征峰作为共有峰,建立了能够使多数化学成分色谱分离的知母药材HPLC-ELSD指纹图谱。结论 该方法简便、可靠,并且同时指认了知母中皂苷类和双苯吡酮类成分,能较全面地反映知母整体性的化学成分特征,可用于全面有效地控制知母的质量。
[Key word]
[Abstract]
Objective To provide the HPLC-ELSD fingerprint analysis method of Anemarrhenae Rhizoma, and to reflect and comprehensively control the quality of Anemarrhenae Rhizoma. Methods The HPLC-ELSD separation was performed on a C8 analytical column (4.6 mm×250 mm, 5 μm) gradient eluted with a mixture consisting of acetonitrile (A) and 0.2% acetic acid-water (B) at a flow rate of 1 mL/min with ELSD detector. Using a linear gradient of 0 min, 5% A; 5 min, 7% A; 5-15 min, 15% A; 15-36 min, 22% A; 36-43 min, 35% A; 43 min, 40% A; 51 min, 50% A; 51-60 min, 100% A. The temperature of column was 25℃. The flow rate of ELSD detector atomizer (air) was 2.6 mL/min. The temperature of the drift tube was 100℃ and the injection volume was 20 μL. Results The fingerprint with better separation effect by using gradient elution method within 60 min was established, and also the 12 peak which are common peak were determined. The most of chemical components of Anemarrhenae Rhizoma were chromatographic separated in this HPLC-ELSD fingerprint. Conclusion The method is simple and reliable, and in this way for the steroidal saponins and flavonoids of Anemarrhenae Rhizoma can be identified at the same time. Moreover, it can fully reflect the characteristics of the chemical composition of Anemarrhenae Rhizoma, therefore it can be used as an effective quality control method for Anemarrhenae Rhizoma.
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[基金项目]
贵州省科技厅联合基金资助(黔科合中药字[2010]LKZ7031)