摘要
目的:建立UPLC-MS/MS同时测定水飞蓟中5个黄酮类化合物(花旗松素、水飞蓟亭、水飞蓟宁、水飞蓟宾B、异水飞蓟宾B)含量的方法。方法:采用Waters ACQUITY Premier CSH C_(18)(50 mm×2.1 mm,1.7µm)色谱柱,以乙腈和0.1%甲酸水溶液为流动相,梯度洗脱,流速0.25 mL·min^(-1),柱温30℃,进样量1µL;采用电喷雾电离源(ESI源),多反应监测(MRM)模式进行负离子检测。结果:5个成分质量浓度在10~200 ng·m L^(-1)范围内线性关系良好,相关系数r均≥0.998;重复性和稳定性良好,RSD均≤5%;平均加样回收率为83.6%~96.0%,RSD≤4.7%。10批次水飞蓟中花旗松素、水飞蓟亭、水飞蓟宁、水飞蓟宾B、异水飞蓟宾B的含量在0.94~1.72、2.70~4.09、0.13~1.46、2.56~5.13、0.27~0.46 mg·g^(-1)。结论:本方法准确、灵敏,稳定性和重复性好,可用于水飞蓟中5个黄酮类化合物的质量控制。
Objective:To establish an UPLCMS/MS method for the simultaneous determination of 5 flavonoids(taxifolin,silicristin,silydianin,silybin B,isosilybin B)in Silybi Fructus.Methods:A Waters ACQUITY Premier CSH C_(18) chromatographic column(50 mm×2.1 mm,1.7μm)was used.The mobile phases consisted of acetonitrile-0.1%formic acid aqueous solution.Gradient elution was performed at a flow rate of 0.25 mL·min^(-1)with a column temperature of 30 C and an injection volume of 1μL.Negative ion detection was carried out using an electrospray ionization(ESI)source in multiple reaction monitoring(MRM)mode.Results:The 5 components exhibited excellent linearity within the concentration range of 10-200 ng·mL-1,with correlation coefficients(r)all above 0.998.The method demonstrated good repeatability and stability,with relative standard deviations(RSD)≤5%.The average recovery rates of spiked samples ranged from 83.6%to 96.0%,with RSDs≤4.7%.The content of taxifolin,silychristin,silydianin,silybin B,isosilybin B were 0.941.72,2.704.09,0.131.46,2.56-5.13,0.270.46 mg·g^(-1),respectively.Conclusion:The method is accurate,sensitive,stable and reproducible,making it suitable for the quality control of the five flavonoids in Silybi Fructus.
作者
张莎莎
蒋俊杰
胡侠
陈文彬
李丽丽
韩超
ZHANG Sha-sha;JIANG Jun-jie;HU Xia;CHEN Wen-bin;LI Li-li;HAN Chao(Comprehensive Technical Service Center of Wenzhou Customs,Wenzhou 325027,China;The 906th Hospital of Chinese People's Liberation Army Joint Logics Support Force,Wenzhou 325000,China;College of Biology and Environmental Engineering,Zhejiang Shuren University,Hangzhou 310015,China)
出处
《药物分析杂志》
北大核心
2025年第12期2060-2066,共7页
Chinese Journal of Pharmaceutical Analysis
基金
浙江省基础公益研究计划项目(LTGN24C200010)。
