UPLC-MS/MS法同时测定金花葵中11个活性成分

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 C₁₈（2.1 mm×100 mm，1.7 μm）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-MS²）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、0.7264~3.632 μg·mL^-1范围内线性关系良好（R² ≥ 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-MS²) were used for quantitative analysis.Results:Good linearity (R² ≥ 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.

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