闪蒸-气相色谱/质谱法同时测定四神丸中8个有效成分

Simultaneous determination of 8 active components in Sishen pills by flash evaporation-gas chromatography/mass spectrometry

目的:建立闪蒸-气相色谱/质谱法(FE-GC/MS)同时测定四神丸中补骨脂素、异补骨脂素、五味子甲素、去氢二异丁香酚、五味子乙素、五味子醇甲、吴茱萸碱和吴茱萸次碱8个有效成分的含量。方法:将四神丸粉末样品置于裂解器中,在300℃下闪蒸后采用GC或GC/MS分析,色谱柱为UA-5(30 m×0.25mm×0.25μm),载气为氦气,程序升温(初始温度50℃,以10℃·min^(-1)升至200℃,再以5℃·min^(-1)升至300℃,10 min),进样口温度300℃,FID(300℃)或质谱检测器(EI离子源,无溶剂延迟,扫描范围m/z 50～600)。结果:8个有效成分达到完全分离,重复性良好,RSD小于6.2%。8个成分在20～10 000 ng范围内线性关系良好,r>0.992,样品加标回收率为92.6%～107.5%。对7批四神丸样品进行了定量分析,并与HPLC法所得结果进行比较,通过五味子醇甲的含量变化及对安五脂素的质谱定性,可鉴别五味子的疑似掺杂。结论:该方法前处理简单,检测灵敏度高,准确可靠,可用于四神丸的质量控制。

Objective:To develop a flash evaporation-gas chromatography/mass spectrometry(FE-GC/MS)method for simultaneous determination of psoralen,isopsoralen,deoxyschizandrin,dehydrodiisoeugenol,γ-Schisandrin,schisandrin,evodiamine and rutaecarpine in Sishen pills.Methods:Powdered Sishen pills was directly added to a sample cup,then evaporated at 300 ℃ and the analytes were analyzed by GC or GC/MS.UA-5 capillary column(30 m×0.25 mm×0.25 μm)was used with temperature programming.The oven temperature was raised from 50℃ to 200 ℃ at a rate of 10 ℃·min-1,then raised to 300 ℃ at a rate of 5 ℃·min-1 and was maintained for 10 min.The injector was set at 300 ℃.FID(temperature was 300 ℃)or mass spectrometry(EI ion source with its scanning at the range of m/z 50-600,and no solvent delay).Results:The 8 components were well separated,and RSD was less than 5.3 %,showing good reproducibility.The calibration curves exhibited good linearity with regression coefficients more than 0.992 at the conc entration range from 20 to 10 000 ng for all the components.The recoveries were 92.6%-107.5%.Finally,the contents of these 8 components in Sishen pills from 7 manufactories samples were analyzed,and the results were compared with those obtained by HPLC method.The Doping of Wuweizi might be detected by the content variation of schisandrin and qualitative analysis of anwuligan.Conclusion:The method was simple,sensitive,accurate,reliable,and could be used for quality control of Sishen pills.