高效液相色谱-质谱联用鉴定黄芩总苷元提取物中黄酮类成分

Identification of Flavonoids from Scutellaria Total Flavonoids Extracts by High Performance Liquid Chromatography-Mass Spectrometry

目的:使用高效液相色谱-四极杆-飞行时间串联质谱(HPLC-Q-TOF/MS)技术,分离鉴定黄芩总苷元提取物中的黄酮类成分,并总结其裂解规律。方法:采用岛津LX-20210330-01 C_(18)(250 mm×4.6 mm,5μm)色谱柱,以0.1%甲酸为流动相A,甲醇-乙腈(50∶50)为流动相B进行梯度洗脱,对黄芩总苷元提取物中的黄酮类成分进行分离,利用电喷雾离子化-四极杆-飞行时间串联质谱高分辨测定各成分母离子及其子离子的准确质量,结合电喷雾离子源正、负离子模式下的质谱信息和色谱保留时间进行结构鉴定。结果及结论:除了黄芩素和汉黄芩素两个已知成分外,从黄芩总苷元提取物中共鉴定出31种黄酮类成分,包括12种苷类与19种苷元,其中有3个化合物为本研究首次鉴定,并分析归纳了黄酮类成分在电喷雾离子源正、负离子模式下的质谱碎片裂解规律。

Objective:To separate and identify flavonoids from Scutellaria total flavonoids extracts by high performance liquid chromatography-quadrupole time-of-flight mass spectrometry(HPLC-Q-TOF/MS),and summarize their fragmentation rules.Methods:The flavonoids in Scutellaria total flavonoids extracts were separated on a C18(250 mm×4.6 mm,5μm)column with gradient elution by 0.1%formic acid as mobile phase A and methanol-acetonitrile(50∶50)as mobile phase B.The exact mass of the parent ion and their product ions of each compound was determined by electrospray-ionization quadrupole time-of-flight mass spectrometry(ESI-Q-TOF/MS).The flavonoids from Scutellaria total flavonoids extracts were identified by ESI-MS information under positive and negative ion modes in combination with chromatographic retention times.Results&Conclusion:In addition to two known compounds,baicalein and wogonin,a total of 31 flavonoids were tentatively identified from Scutellaria total flavonoids extracts,including 12 glycosides and 19 aglycones.Among them,three compounds were identified for the first time in this study,and the fragmentation rules of flavonoids under ESI positive and negative ion modes were analyzed and summarized.