摘要
采用高效液相色谱-大气压化学电离质谱法(HPLC-APCI/MS)和直接进样的电喷雾串联质谱法(ESI-MS^2)分析大青叶乙酸乙酯、正丁醇和95%乙醇提取物的化学成分。采用Kromasil C18分析柱(4.6 mm×250 mm×5μm),以0.15%乙酸/水-甲醇为流动相进行线性梯度洗脱,流速0.8 mL/min,柱温25℃;采用全波长扫描紫外检测器,检测波长分别为254 nm和265 nm;采用大气压化学电离源和电喷雾电离源,在正、负两种离子模式下进行检测。结果表明,在大青叶乙酸乙酯、正丁醇和95%乙醇提取物中共鉴别出39种化合物,包括生物碱类、有机酸类、核苷嘌呤类、氨基酸类、黄酮类、糖类、卟啉类以及含硫类成分化合物。采用铁离子还原能力法(FRAP)对大青叶的抗氧化活性进行评价,并用自由基清除能力法验证FRAP法的测试结果。抗氧化活性评价结果表明,大青叶抗氧化活性部位主要集中在极性较低的化学组分中,吲哚类、奎唑酮类和有机酸类化合物是其主要有效成分。该方法快捷、灵敏,适用于中药化学成分分析和抗氧化活性评价。
High performance liquid chromatography-atmospheric pressure chemical ionization/mass spectrometry(HPLC-APCI/MS) and electrospray ionization tandem mass spectrometry(ESI-MS^2) were applied to analyze the chemical constituents from acetate, n-BuOH and 95% ethanol extracts of Isatidis Folium. The separation was performed on a Kromasil C18 column(4.6 mm×250 mm×5 μm) with the gradient of 0.15% acetic acid/water-methanol as mobile phase with a flow rate of 0.8 mL/min at 25 ℃. The UV spectra were obtained by a diode array detector(DAD) under the detection wavelength at 254 nm and 265 nm. In order to get exact data of MS and MS^2 spectra, the atmosphere pressure chemical ionization ion source(APCI) and electrospray ionization ion source(ESI) in both positive and negative mode were utilized. Up to date, thirty-nine different compounds were identified from the crude extracts, including alkaloids, organic acids, nucleosides and purines, amino acids, flavones, carbohydrates, porphyrin and epigoitrin. Meanwhile, the antioxidant activity of the extracts from Radix Isatidis were successfully estimated by the ferric reducing antioxidant power(FRAP) and radical scavenging(DPPH) methods. The results of the antioxidant activities indicated that the compositions of antioxidant activity were mainly existed in the small polarity part. Indoles, quinazolinones, organic acids and porphyrins might be the main antioxidative constituents of Radix Isatidis. This method is rapid and sensitive that can be used for analyzing the chemical compositions and antioxidant activities of traditional Chinese medicine.
作者
闫峻
顾娟
冯硕
姬瑞芳
全庆华
刘永刚
YAN Jun;GU Juan;FENG Shuo;JI Ruifang;QUAN Qing-hua;LIU Yong-gang(Beijing Research Institute of Uranium Geology,Beijing 100029,China;Chin-Japan Friendship Hospital,Beijing 100029,China;Beijing University of Uranium Chinese Medicine,Beijing 100029,China)
出处
《质谱学报》
EI
CAS
CSCD
北大核心
2019年第4期381-390,I0004,共11页
Journal of Chinese Mass Spectrometry Society
基金
国家自然科学基金项目(81703640)资助