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目的:通过LC-TOF/MS快速鉴定女贞子4种环烯醚萜苷类化合物(特女贞苷、新女贞苷、橄榄苦苷、女贞苷)模拟清蒸品的化学成分,探讨女贞子蒸制过程中环烯醚萜苷类成分的转化机制。方法:色谱条件为流动相乙腈(A)-0.1%甲酸溶液(B)梯度洗脱(0~5 min,7%~12%A;5~20 min,12%~25%A;20~30 min,25%~40%A;30~35 min,40%~100%A),流速0.2 m L·min-1,柱温25℃,进样量3μL,检测波长240 nm;质谱使用Agilent 6230型LC-TOF/MS联用系统,在ESI/MS正离子模式下采集数据。通过对照品定位、质谱数据及文献参照分析4种环烯醚萜苷类化合物模拟清蒸品的化学成分。结果:4种环烯醚萜苷类化合物模拟清蒸品中均检出了橄榄酸;特女贞苷模拟清蒸品中还检出红景天苷和2种特女贞苷异构体;新女贞苷模拟清蒸品中鉴定出了3,4-二羟基苯乙基-β-D-葡萄糖苷;橄榄苦苷和女贞苷模拟清蒸品中分别检出其各自的苷元羟基酪醇和酪醇。结论:女贞子中环烯醚萜苷类成分性质不稳定,加水、加热可使其水解生成次级苷或者苷元,特女贞苷在模拟炮制过程中可转化为其异构体。女贞子酒蒸后补肝肾药效增强与其环烯醚萜苷类成分水解密切相关。
OBJECTIVE: To rapidly identify the chemical constituents of four kinds of iridoid glycosides (especially rosette, new virginia, oleuropein and virginia) in Ligustrum lucidum by LC-TOF / MS, Transformation Mechanism of Iridoid Glycosides in Fructus. Methods: The chromatographic conditions were gradient elution (0-5 min, 7-12% A; 5-20 min, 12-25% A; 20-30 min, 25% -40% A, 30-35 min, 40% -100% A) at a flow rate of 0.2 m L · min-1 at a column temperature of 25 ℃ with a detection wavelength of 240 nm. LC-TOF / MS system to collect data in ESI / MS positive mode. The chemical composition of the four iridoid glycosides was simulated by reference standard, mass spectrometry data and literature references. Results: Four kinds of iridoid glycosides were detected in the simulation of steamed savory products are all acid; special virtuosin simulated steamed also detected in the salidroside and two kinds of extra virginia isomers; new female 3,4-Dihydroxy-phenethyl-β-D-glucoside was identified in the simulant simulant steamed product; and their respective aglycones and tyrosol were detected in simulated steamed products of oleuropein and virginia, respectively . CONCLUSION: Iridoid glycosides in Fructus Ligustri Lucidi are unstable in nature. When heated, they can be hydrolyzed to form secondary or aglycones, which can be converted into their isomers during the simulation process. Ligustrum lucidum wine after liver and kidney enhanced efficacy of its iridoid glycoside component of the hydrolysis is closely related.