摘要
目的:建立山茱萸药材及其制剂的鉴别方法。方法:采用液-质(LC-MS)联用法。LC条件:色谱柱为HypersilODSC18(150mm×2.1mm,5μm),柱温为30℃,流动相为甲醇-10mmol·L-1醋酸铵溶液(84∶16),流速为0.2mL·min-1。MS条件:离子源为ESI,负离子扫描模式,鞘气流速为1.5L·min-1,辅气流速为0.45L·min-1,喷雾电压为4.5kV,高温毛细管温度为350℃,扫描范围为110～600amu。结果:山茱萸脂溶性成分熊果酸和齐墩果酸的LC-MS三级MS图分离效果好,结果稳定;建立了10批山茱萸药材脂溶性成分的三级MS图,并对其制剂进行了鉴别。结论:山茱萸脂溶性成分的三级碎片峰可用于山茱萸药材及其制剂的鉴别。
OBJECTIVE： To establish a method for identification of Comus officinalis and its Preparations. METHODS： LC-MS method was adopted. The separation was performed on Hypersil C18 column （150 mm×2.1 mm, 5 um） with a mobile phase of methanol-acetic acid（84 ： 16） at a flow rate of 0.2 mL.min^-1. The column temperature was set at 30℃. Mass spectra were equipped with an electrospray ionization （ESI） source with negative ion detection model as ion scanning. The conditions of determination were sheath gas flow rate of 1.5 L. min^-1, sweep gas flow rate of 0.45 L. min^-1, spraying voltage of 4.5 kV, high temperature capillary temperature of 350℃ and scan range of 110-600 amu. RESULTS： The three-level mass spectrometry of the ursolic acid and oleanolic acid was well separated. The results were stable. Three-level mass spectrometry of ursolic acid and oleanolic acid were established and identification of C of/icinalis preparations was carded out.CONCLUSION： Three-level fragment peaks of fat-soluble constituents of C. officinalis can be used for indentification of C officinalis and its preparations.
出处
《中国药房》
CAS
CSCD
北大核心
2010年第11期1004-1006,共3页
China Pharmacy
基金
国家科技支撑计划子课题(2006BAI09B05-8)
