采用液相色谱-串联质谱法对农吉利中黄酮化合物进行定性和定量分析.农吉利干药材粉碎后,用甲醇提取,提取液经D101大孔吸附树脂净化后,以UltimateTM C18色谱柱为固定相,以甲醇-0.5%(φ)乙酸混合溶液为流动相进行梯度洗脱,采用电喷雾离子源,分别在正离子和负离子扫描模式下对主要特征碎片离子进行解析.结果表明:提取液中含有牡荆苷、异牡荆苷、荭草苷、异荭草苷和金雀花苷等黄酮类化合物.荭草苷、异荭草苷、牡荆苷和异牡荆苷的质量浓度在一定范围内与其峰面积呈线性关系,检出限(3S/N)分别为50.2,40.5,52.1,42.1 μg·L-1.方法应用于农吉利药材的分析,加标回收率在96.0%~103%之间,测定值的相对标准偏差(n=5)小于3.0%.

A method of LC-MS/MS was used for qualitative and quantitative analysis of flavonoids in Crotalaria sessiliflora L.. The sample was smashed and extracted with methanol,and then purified with D101 macroporous resin. UltimateTM C18 column was used as stationary phase and the mixture of methanol and 0.5% (φ) acetic acid was used as mobile phase for gradient elution. ESI was adopted in MS/MS. The main characteristic fragment ions were analyzed in the positive and negative ion scan mode. Vitexin,isovitexin,orientin,isoorientin and trematin were detected based on MS/MS data. Linear relationship were found between the peak area and the mass concentration of orientin,isoorientin,vitexin,isovitexin in a certain range,with detection limits (3S/N) of 50.2,40.5,52.1,42.1 μg·L-1,respectively. The method was applied for analysis of Crotalaria sessiliflora L. samples,giving recoveries determined by standard addition method in the range of 96.0%-103% with RSD (n=5) less than 3.0%.