UPLC-MS/MS法同时测定金花葵中11个活性成分  

Simultaneous determination of 11 active components in Aurea helianthus by UPLC-MS/MS

作　　者：张迪文 马开[1] 田萍 ZHANG Di-wen;MA Kai;TIAN Ping(Henan Province Chinese Medicine Research Institute,Zhengzhou 450004,China)

机构地区：[1]河南省中医药研究院,郑州450004

出　　处：《药物分析杂志》2019年第5期780-786,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：河南省基础与前沿技术研究项目(112300410063)

摘　　要：目的:建立UPLC-MS/MS法同时测定金花葵中11个活性成分(没食子酸、原儿茶酸、绿原酸、咖啡酸、芦丁、金丝桃苷、异槲皮苷、棉皮素、槲皮素-3’-O-葡萄糖苷、杨梅素、槲皮素)的含量。方法:色谱条件:采用Waters ACQUITY BEN C_(18)(2.1 mm×100 mm,1.7μm)色谱柱,以0.05%甲酸水-乙腈为流动相,梯度洗脱,流速为0.2 mL·min^(-1),柱温为30℃。质谱条件:采用电喷雾电离源(ESI),正负离子全扫模式(Full MS/dd-MS^2)扫描进行定量分析。结果:金花葵中没食子酸、原儿茶酸、绿原酸、咖啡酸、芦丁、金丝桃苷、异槲皮苷、棉皮素、槲皮素-3’-O-葡萄糖苷、杨梅素、槲皮素的质量浓度分别在0.030 64～0.153 2、0.044 00～0.220 0、0.144 0～0.720 0、0.026 64～0.133 2、6.352～31.76、8.704～43.52、5.728～28.64、24.30～121.5、5.824～29.12、2.248～11.24、0.7264～3.632μg·mL^(-1)范围内线性关系良好(R^2≥0.999 1),精密度、重复性、稳定性均良好,平均加样回收率在94.5%～100.7%之间,RSD≤3.2%;8批金花葵样品中上述11个活性成分的含量范围分别为0.005～0.049、0.008～0.122、0.032～0.267、0.012～0.033、2.439～4.214、4.904～7.216、3.915～5.945、12.126～17.518、4.006～5.423、0.573～1.753、0.186～1.243 mg·g^(-1)。结论:该方法可用于金花葵药材的质量控制。Objective:To establish an ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of 11 active components(gallic acid,protocatechuic acid,chlorogenic acid,caffeic acid,rutin,hyperin,isoquercitrin,hibifolin,quercetin-3’-O-glucoside,myricetin and quercetin)in Aurea helianthus.Methods:Chromatographic conditions:The chromatographic column was Waters ACQUITY BEN C18(2.1 mm×100 mm,1.7 μm).The mobile phase was composed of 0.05% formic acid water(A)and acetonitrile(B)in gradient elution at a flow rate of 0.20 mL·min^-1 and the column temperature was set at 30 ℃.Mass spectrum conditions:The electrospray ionization source(ESI)and positive and negative ion monitoring mode(Full MS/dd-MS^2)were used for quantitative analysis.Results:Good linearity(R^2 ≥0.999 1)was achieved for gallic acid,protocatechuic acid,chlorogenic acid,caffeic acid,rutin,hyperin,isoquercitrin,hibifolin,quercetin-3’-O-glucoside,myricetin and quercetin in the range of 0.030 64-0.153 2,0.044 00-0.220 0,0.144 0-0.720 0,0.026 64-0.133 2,6.352-31.76,8.704-43.52,5.728-28.64,24.30-121.5,5.824-29.12,2.248-11.24 and 0.726 4-3.632 μg·mL^-1,respectively.The precision,repeatability,and stability were good in this method.The average recoveries varied between 94.5% and 100.7% with RSDs ≤ 3.2%.And the average contents of 11 active components in 8 batches of Aurea helianthus were 0.005-0.049,0.008-0.122,0.032-0.267,0.012-0.033,2.439-4.214,4.904-7.216,3.915-5.945,12.126-17.518,4.006-5.423,0.573-1.753 and 0.186-1.243 mg·g^-1.Conclusion:This method can be used for the quality control of Aurea helianthus.

关 键 词：UPLC-MS/MS 金花葵 没食子酸 原儿茶酸 绿原酸 咖啡酸 芦丁 金丝桃苷 异槲皮苷 棉皮素 槲皮素-3’-O-葡萄糖苷 杨梅素 槲皮素 

分 类 号：R917[医药卫生—药物分析学]