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目的:建立竹节参药材HPLC-ELSD液相指纹图谱,分离纯化鉴定其主要特征峰的单体化合物,客观评价竹节参内在质量差异。方法:采用高效液相色谱-蒸发光散射检测器(HPLC-ELSD),梯度洗脱,测定了10批竹节参样品。色谱条件为YMC-pack ODS-AQ色谱柱(4.6 mm×250 mm,5μm),乙腈(A)-0.5%乙酸水溶液(B)为流动相,梯度洗脱(0~5 min,20%~40%A;5~20 min,40%~40%A),流速为1.0 mL.min-1,柱温30℃。ELSD检测器:漂移管温度为40℃,氮气释放压力为33 Psi。通过采用反复硅胶柱色谱和半制备HPLC的方法分离纯化竹节参的化学成分,并根据理化性质和波谱数据进行结构鉴定。结果:建立了10批竹节参样品HPLC-ELSD指纹图谱,分离纯化鉴定了5个主要化学成分,分别为人参皂苷Re,竹节参皂苷Ⅳ,Ⅳa,Ⅴ,Pjs-2。结论:综合竹节参指纹图谱和化学成分分析,能较全面的表征不同产地竹节参内在成分的差异,为竹节参内在质量评价提供依据。
OBJECTIVE: To establish HPLC-ELSD liquid-phase fingerprinting (HPLC-ELSD) fingerprinting of Panax japonicus, and to isolate and purify the main compounds identified by HPLC. Methods: Ten batches of bamboo ginseng samples were determined by HPLC-ELSD and gradient elution. The chromatographic conditions were as follows: YMC-pack ODS-AQ column (4.6 mm × 250 mm, 5 μm), acetonitrile-A0.5% acetic acid aqueous solution % A; 5 ~ 20 min, 40% ~ 40% A), the flow rate was 1.0 mL.min-1, the column temperature was 30 ℃. ELSD detector: Drift tube temperature is 40 ° C and nitrogen release pressure is 33 Psi. The chemical constituents of P. japonicus were isolated and purified by repeated silica gel column chromatography and semi-preparative HPLC. The structures were elucidated on the basis of physico-chemical properties and spectral data. Results: Ten batches of Panax japonicus samples were established by HPLC-ELSD. Five major chemical constituents were isolated and identified, which were ginsenoside Ⅳ, Ⅳa, Ⅴ and pjs-2. Conclusion: Based on the fingerprinting and chemical composition analysis of fingerprints, the difference in the intrinsic components of bamboo siphon from different areas can be fully characterized, which provides the basis for evaluating the intrinsic quality of siphonoid.