SPME-GC/MS结合保留指数分析当归及妇科千金片和胶囊中的挥发性成分

Analysis of volatile compounds in Angelicae Sinensis Radix,Fukeqianjin tablets and capsules by SPME-GC/MS with retention index

目的:采用固相微萃取结合气相色谱/质谱联用技术(SPME-GC/MS)提取、鉴定当归药材中的挥发性成分,并用保留指数(RI)进一步确认。方法:通过优化萃取头、平衡温度、萃取时间等条件,建立当归SPME-GC/MS的测定方法,采用DB-5石英毛细管柱(30 m×0.25 mm,0.25μm),PDMS/DVB萃取头(65μm),在分流比10∶1,载气流速为1 mL·min^−1的条件下,按照设定的程序升温条件运行,用峰面积归一化法进行半定量分析,并运用主成分分析进一步研究妇科千金片和胶囊中当归差异性挥发成分。结果:从当归中检测出94个挥发性成分,在不同批次的妇科千金片及胶囊中检测到41个当归中存在的挥发性成分,片剂和胶囊剂中所测挥发性成分的种类和含量存在一定的差异,4-羟基-3-甲氧基苯乙酮、β-红没药烯、β-金合欢烯、十四碳烯、1-(2,4-二甲基苯基)-1-丙酮、E-丁烯基苯酞、当归酸为评价二者的差异性成分。结论:SPME-GC/MS适用于当归及其制剂中挥发性成分的定性与半定量分析。妇科千金片和胶囊中的挥发性物质可能是其药效物质基础的一部分。

Objective:To extract and identify volatile compounds in Angelicae Sinensis Radix using solidphase micro-extraction combined with gas-chromatography/mass-spectrum(SPME-GC/MS),a new method established by optimizing different extraction fibers,equilibrium temperature and extraction time.Methods:DB-5 quartz capillary column(30 m×0.25 mm,0.25μm)and PDMS/DVB fiber(65μm)were used in the established method.The shunt ratio was 10∶1,the carrier gas flow rate was 1 mL·min^-1.Then analysis was performed according to the set program heating conditions.The volatile compounds were analyzed qualitatively and semi-quantitatively with retention index(RI)and area normalization method,and the symbolic volatile compounds of Angelicae Sinensis Radix existed in Fukeqianjin tablets and capsules could be investigated by using principal components analysis(PCA).Results:In this work,94 volatile compounds were detected from Angelicae Sinensis Radix,41 of which with some differences in varieties and contents were identified from different batches of Fukeqianjin tablets and capsules.4-hydroxy-3-methylacetophenone,β-bisabolene,cis-β-farnesene,tetradecane,1-(2,4-dimethylphenyl)-1-propanone,E-butylidenephthalide and angelic acid could be considered as symbolic compounds to evaluate the stability of these two kinds of dosage forms.Conclusion:These results indicate that SPME-GC/MS is suitable for qualitative and semi-quantitative analysis of Angelicae Sinensis Radix and its preparations.The volatile compounds may be the experiment references for therapeutic effects.