HPLC-VWD-Q-TOF-MS/MS法定性与定量分析枳实栀子豉汤成分

Qualitative and quantitative analysis of constituents in Zhishi Zhizi Chi Decoction by HPLC-VWD-Q-TOF-MS/MS

目的采用HPLC-Q-TOF-MS/MS法快速鉴定枳实栀子豉汤化学成分和HPLC-VWD法同时测定枳实栀子豉汤中的6种成分。方法采用HPLC-Q-TOF-MS/MS技术,在正、负离子模式下分别定性分析,借助PeakView分析软件,比对部分标准品,同时参考相关文献,分析推断枳实栀子豉汤中的化学成分。采用HPLC-VWD法同时定量枳实栀子豉汤的6种成分(京尼平龙胆双糖苷、栀子苷、大豆苷、柚皮苷、橙皮苷、新橙皮苷)。结果从中共鉴定出38个化合物,包括枳实15个化合物、栀子14个化合物、淡豆豉10个化合物,1个化合物为栀子与淡豆豉共有。6种成分在各自范围内线性关系良好(r>0.9990);加样回收率98.44%~101.32%;RSD 0.47%~1.68%。结论该方法稳定可靠,可用于枳实栀子豉汤的质量控制。

AIM To establish HPLC-Q-TOF-MS/MS and HPLC-VWD methods for rapid identification of constituents from Zhishi Zhizi Chi Decoction and simultaneous determination of the six constituents.METHODS The HPLC-Q-TOF-MS/MS was used for qualititive analysis in both positive and negative ion modes.With the help of PeakView software,the chemical constituents in Zhishi Zhizi Chi Decoction were analyzed and inferred by comparing with standards and referring to relevant literature.HPLC-VWD was used to simultaneous determination of six constituents,including genipin-1-β-D-gentiobioside,geniposide,daidzin,naringin,hesperidin,neohesperidin.RESULTS Thirty-eight constituents were identified in Zhishi Zhizi Chi Decoction,fifteen compounds in Aurantii Fructus Immaturus,fourteen compounds in Gardeniae Fructus,ten compounds in Sojae Semen Praeparatum,Fructus Gardeniae and Sojae Semen Praeparatum shared one compound.Six constituents showed good linear relationships within their own ranges(r>0.9990),whose average recoveries were 98.44%-101.32%with the RSDs of 0.47%-1.68%.CONCLUSION This method is stable and reliable,and can be used for the quality control of Zhishi Zhizi Chi Decoction.