摘要
将实时直接分析(DART)离子源与高分辨率质谱Orbitrap联用,建立了一种对黄芩药材进行快速定性定量分析的方法。定性分析时,对其中的化学成分进行标准品比对和二级质谱确证,同时参考相应文献进行确认。定量分析时,采用Full MS-SIM及Targeted-MS2扫描方式采集信号,Targeted-MS2扫描方式下分别对黄芩素和汉黄芩素的母离子和子离子的提取离子流图积分,通过峰面积计算含量。在黄芩药材中检出黄芩素、汉黄芩素、韧黄芩素Ⅱ、二羟基-二甲氧基黄酮、5,7,2',5'-四羟基-8,6'-二甲氧基黄酮和SkullcapflavonⅡ的[M+H]+峰。定量分析结果显示,黄芩素(m/z 271.06→123.01)的线性范围为49.7~447.3 ng,相关系数(r2)为0.995,平均加标回收率为87.0%;汉黄芩素(m/z 285.07→270.05)的线性范围为50.0~350ng,r2为0.995,平均加标回收率为66.0%。该方法可用于黄芩药材的快速定性检测和定量分析。
A DART coupled with Orbitrap mass spectrometric method was developed for the qualita- tive and quantitative analyses of scutellaria radix. The component was identified by comparing with standard component and the report of relative researches as well as the full scan spectra and secondary spectra. In quantitative analysis, the Full MS -SIM and Targeted -MS2 mode was applied to obtain the mass spectrum, extract ion chromatography based on the parents ion and the product ion of baica- lein(m/z 271.06→123.01 ) and wogonin(m/z 285.07→270.05 ) were used for quantitative analysis in the Targeted - MS2 mode. The signals of baicalein, wogonin, Skullcapflavon Ⅱ and other compo- nents were observed in the mass spectra of scutellaria radix. The linear ranges of baiealein and wogo- nin were 49.7 -447.3 ng(r2 = 0. 995 ) and 50. 0 - 350 ng(r2 = 0. 995) , respectively. Their aver- age recoveries were 87.0% and 66.0% , respectively. This method is suitable for the rapid analysis of scutellaria radix and other traditional Chinese herbal medicines.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第7期859-863,共5页
Journal of Instrumental Analysis
基金
农业部公益性行业基金(201303111)