UHPLC-MS/MS法同时测定枳实薤白桂枝汤中10种成分

Simultaneous determination of 10 components in Zhishi Xiebai Guizhi Decoction by UHPLC-MS/MS

关键词:  超高效液相色谱-质谱联用  枳实薤白桂枝汤  含量测定  化学成分

Key words:  UHPLC-MS/MS  Zhishi Xiebai Guizhi Decotion  content determination  chemical composition

摘要:

[目的] 建立超高效液相色谱-质谱联用（UHPLC-MS/MS）方法同时测定枳实薤白桂枝汤中槲皮素、芹菜素、原儿茶酸、木犀草素、紫丁香苷、阿魏酸、柚皮苷、厚朴酚、橙皮苷、新橙皮苷的含量。[方法] 采用Welchultimate XB-C18色谱柱（2.1 mm×100 mm，3 μm），以0.1%甲酸水-乙腈为流动相，梯度洗脱，进样量为3 μL，流速为0.2 mL/min，柱温40 ℃。采用电喷雾离子源（ESI），正负离子切换模式，多反应检测（MRM）模式。[结果] 枳实薤白桂枝汤颗粒中10种成分在各自范围内线性关系良好（r＞0.995），精密度、稳定性及重复性实验的相对标准偏差（RSD）均小于2.86%，加样回收率均在97.68%~101.66%。[结论] 该方法简便快捷、结果准确可靠，可用于枳实薤白桂枝汤颗粒的质量控制。

Abstract:

[Objective] To establish a method for the determination of quercetin，apigenin，protocatechuic acid，luteolin，syringin，ferulic acid，naringin，magnolol，hesperidin and neohesperidin in Zhishi Xiebai Guizhi Decotion by UPHLC-MS/MS to provide a reference for their quality control. [Methods] The constituents separation was carried on Welchultimate XB-C₁₈ column （2.1 mm×100 mm，3 μm） with a mobile phrase of 0.1% formic acid in water and acetonitrile，gradient elution，the injection volume was 3 μL，the flow rate was 0.2 mL/min，and the column temperature was 40 ℃. ESI ion source，positive and negative ion switching mode，multiple reaction detection （MRM） mode were employed. [Results] The contents of 10 components in Zhishi Xiebai Guizhi Decotion were measured. The results of the methodological investigation of the quantitative analysis conditions were good（r>0.995），the RSD of the precision，stability and reproducibility tests were less than 2.86%，and the recovery of the spiked samples were between 97.68% and 101.66%. [Conclusion] The method is simple，rapid，accurate and reliable，and can be used for the quality control of Zhishi Xiebai Guizhi Decotion.