UPLC-MS/MS法对5个产地黑果枸杞指标成分检测研究

UPLC-MS/MS method on index composition of black fruit in 5 countries of origin

目的对5个产地黑果枸杞指标成分进行定性定量分析。方法采用UPLC-MS/MS法,色谱柱为Agilent Eclipse Plus-C18(150 mm×2.1 mm,1.8-Micron),流动相为以0.1%甲酸-甲醇,梯度洗脱,柱温25℃,在电喷雾(ESI)正负离子模式下,用多重反应扫描模式进行检测。结果没食子酸在2~100μg/mL,儿茶素在0.5~50μg/mL,芦丁在0.1~200μg/mL,飞燕草色素在20~150μg/mL,线性关系良好(r>0.997),精密度在RSD在1.7%~2.7%,重复性RSD在2.02%~2.73%,平均回收率为98.5%~99.8%。结论该检测方法操作简便、快速准确、选择性强,适用于黑果枸杞中指标性成分的测定。

Objective To qualitatively and quantitatively analyze the index component of L.ruthenicum by UPLC-MS/MS.Methods L.ruthenicum was extracted and passed through the microporous filter membrane.UPLC-MS/MS was used with Agilent Eclipse plus-C18(150 mm×2.1 mm,1.8micron)chromatographic column,and the column temperature was at 25℃.0.1%carboxylic acid and methanol were used as mobile phases for gradient elution.In electrospray(ESI)positive and negative ion mode,with multiple reaction scan mode monitoring.Results The calibration curves covered the range of 2-100μg/mL,0.5-50μg/mL,0.1-200μg/mL and 20-150μg/mLfor gallic acid,catechin,rutin and delphinidin respectively,and the correlation coefcients(r)were all greater than 0.997.The RSD of precision,repeatability and average recovery were 1.7%-2.7%,2.02%-2.73%and 98.5%-99.8%respectively.Conclusion The detection method is simple,accurate,fast and selective,and is suitable for the determination of the index components in Lycium ruthenicum.