UPLC-MS/MS法同时测定经典方剂槐花散中7个成分含量  

Simultaneous determination of 7 components in classic formula Huaihua powder by UPLC-MS/MS

作　　者：师艺玮 王洪玲 黄慧莲 高燕萍 李娜芝 钟国跃 梁健 SHI Yi-wei;WANG Hong-ling;HUANG Hui-lian;GAO Yan-ping;LI Na-zhi;ZHONG Guo-yue;LIANG Jian(Research Center for Traditional Chinese Medicine Resources and Ethnic Minority Medicine,Jiangxi University of Chinese Medicine,Nanchang 330004,China)

机构地区：[1]江西中医药大学中药资源与民族药研究中心,南昌330004

出　　处：《药物分析杂志》2023年第2期219-226,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金项目(81560641);江西自然科学基金项目(20192ACB20016)。

摘　　要：目的:建立超高效液相色谱串联质谱(UPLC-MS/MS)法同时测定经典名方槐花散中芦丁、胡薄荷酮、川陈皮素、柚皮苷、槲皮苷、新橙皮苷、槲皮素7个有效成分的含量。方法:采用ACQUITY UPLC HSS T3C18色谱柱(100 mm×2.1 mm,1.8μm),以0.1%甲酸水(A)-甲醇(B)为流动相进行梯度洗脱,流速为0.4 mL·min^(-1),柱温为35℃。质谱采用电喷雾离子化(ESI)源,正负离子模式,雾化气流速为3 L·min^(-1),加热气流速为10 L·min^(-1),滞留时间为45 ms,离子源温度为300℃,加热块温度为400℃,脱溶剂管温度为250℃,干燥气流速为10 L·min^(-1);多反应监测模式(MRM)进行定量分析,其中芦丁、胡薄荷酮、川陈皮素采用正离子模式,监测离子对为m/z 611.15/303.00、153.15/81.10、403.15/373.10;柚皮苷、槲皮苷、新橙皮苷和槲皮素采用负离子模式,监测离子对为m/z 579.15/271.15、447.10/300.15、609.15/301.15、301.05/151.05。结果:槐花散中芦丁、胡薄荷酮、川陈皮素、柚皮苷、槲皮苷、新橙皮苷、槲皮素7个有效成分在各自线性范围内线性关系良好,相关系数均>0.9995;精密度、稳定性、重复性试验的RSD均<5.0%;平均回收率分别为97.7%、103.3%、92.3%、100.7%、101.5%、101.0%、100.2%,RSD均<5.0%。6批槐花散中上述7个成分的含量范围分别为44.30~47.00、2.01~2.10、0.31~0.33、18.53~19.80、0.79~0.85、17.64~18.57、1.29~1.35 mg·g^(-1)。结论:该方法快速、灵敏,专属性高,可为槐花散的质量控制提供方法,并为该方的药效学及药代动力学研究提供参考。Objective:To develop an UPLC-MS/MS method for the simultaneous determination of seven activecomponents in Huaihua powder,including rutin,(+)-R-pulegone,nobiletin,naringoside,quercitrin,neohesperidin and quercetin.Methods:An ACQUITY UPLC HSS T3C18(100 mm×2.1 mm,1.8μm)column was used with 0.1%formic acid in water(A)and methanol(B)as mobile phases.A gradient elution was employed with flow rate of 0.4 mL·min^(-1)and column temperature of 35℃.Electrospray ionization(ESI)source was used.Samples were determined in both positive and negative ion modes.MS parameters were 3 L·min^(-1)for nebuliser gas flow,10 L·min^(-1)for heater gas flow,45 ms for dwell time,300℃for source temperature,400℃for heater block temperature,250℃for desolvation tube temperature,and 10 L·min^(-1)for dry gas flow.Multiple-reaction monitoring(MRM)was used to perform mass spectrometric quantification.Rutin,(+)-R-pulegone and nobiletin were measured by precursor/product pairs of m/z 611.15/303.00,153.15/81.10 and 403.15/373.10 in positive ion mode.Naringoside,quercitrin,neohesperidin and quercetin were measured by precursor/product pairs of m/z 579.15/271.15,447.10/300.15,609.15/301.15,301.05/151.05 in negative ion mode.Results:Rutin,(+)-R-pulegone,nobiletin,naringoside,quercitrin,neohesperidin and quercetin had good linearity in their respective linear ranges with all linear correlation coefficients greater than 0.9995 and RSDs of the precision,repeatability and stability less than 5.0%.The average recoveries were 97.7%,103.3%,92.3%,100.7%,101.5%,101.0%and 100.2%,respectively,with RSDs lower than 5.0%.The contents ranges of rutin,(+)-R-pulegone,nobiletin,naringoside,quercitrin,neohesperidin and quercetin in 6 batches of Huaihua powder were 44.30-47.00,2.01-2.10,0.31-0.33,18.53-19.80,0.79-0.85,17.64-18.57 and 1.29-1.35 mg·g^(-1).Conclusion:The proposed method is rapid,sensitive and specific,which could offer an analytical method for the quality control of Huaihua powder,reference and insights for its pharmacodynamic and pharmacokinetic

关 键 词：槐花散 经典名方 含量测定 液质联用 质量控制 芦丁 胡薄荷酮 川陈皮素 柚皮苷 槲皮苷 新橙皮苷 槲皮素 

分 类 号：R917[医药卫生—药物分析学]