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目的:对女贞子中主要药用成分进行定性分析,用电喷雾质谱法探究人血清白蛋白与齐墩果酸相互作用。方法:定性分析采用高效液相色谱电喷雾高分辨质谱(HPLC-ESI-MS)法,色谱柱使用Agilent ZORBAX Eclipse XDB-C18柱(2.1×150 mm,5-Micron),流动相为甲醇(A)-0.1%乙酸水溶液(B),梯度洗脱:0~30 min 10%-90%A,30~40 min 90%A,40-60 min 90%~10%A,柱温:30℃,进样量:1μL,流速:0.2 m L·min-1,女贞子乙醇提取物采用HPLC-ESI-MS负离子检测模式。结果:采用HPLC-ESI-MS定性地检测了女贞子乙醇超声提取液,鉴定出9种有效成分(齐墩果酸、红景天苷、特女贞苷、橄榄苦苷、芹菜素、委陵菜酸、2α-羟基熊果酸、2α-羟基齐墩果酸和19α-羟基-3-乙酰乌索酸)。电喷雾质谱观测到齐墩果酸能与人血清白蛋白形成较为稳定的1:1蛋白质复合物,其结合常数为1.63×104L·mol-1。结论:该方法定性分析了女贞子乙醇提取物中主要药用成分,首次用电喷雾质谱法研究了人血清白蛋白与齐墩果酸的相互作用,从分子水平上揭示了齐墩果酸与人血清白蛋白相互作用的质谱信息。
OBJECTIVE: To qualitatively analyze the main medicinal components in Ligustrum lucidum and to study the interaction between human serum albumin and oleanolic acid by electrospray ionization mass spectrometry. METHODS: Qualitative analysis was performed on a high performance liquid chromatography-electrospray ionization mass spectrometry (HPLC-ESI-MS) column using an Agilent ZORBAX Eclipse XDB-C18 column (2.1 × 150 mm, 5-Micron) ) - 0.1% acetic acid in water (B), gradient elution: 0-30 min 10% -90% A, 30-40 min 90% A, 40-60 min 90% -10% Injection volume: 1μL, flow rate: 0.2 m L · min-1, Ligustrum lucidum ethanol extract by HPLC-ESI-MS negative ion detection mode. Results: The ultrasonic extraction of Ligustrum lucidum ethanol was qualitatively detected by HPLC-ESI-MS. Nine active ingredients were identified (oleanolic acid, salidroside, estrogenin, oleuropein, apigenin, Xanthic acid, 2α-hydroxy ursolic acid, 2α-hydroxy oleanolic acid and 19α-hydroxy-3-acetoxystearic acid). Electrospray ionization mass spectrometry showed that oleanolic acid could form a stable 1: 1 protein complex with human serum albumin with a binding constant of 1.63 × 104 L · mol -1. Conclusion: This method qualitatively analyzed the main medicinal components in ethanol extract of Ligustrum lucidum, and the first time the interaction between human serum albumin and oleanolic acid was studied by electrospray ionization mass spectrometry. From the molecular level it was revealed that oleanolic acid Mass Spectrometry Information Interaction with Human Serum Albumin.