UPLC-MS/MS法同时测定香青兰中6个活性成分的含量  

Simultaneous determination of 6 active ingredients in Dracocephalum moldavica L.by UPLC-MS/MS

作　　者：陈洁 CHEN Jie(The Third People’s Hospital of Haikou,Haikou 571100,China)

机构地区：[1]海口市第三人民医院,海口571100

出　　处：《药物分析杂志》2020年第11期1986-1993,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立超高效液相色谱串联三重四极杆质谱(UPLC-MS/MS)法同时测定香青兰药材中熊果酸、齐墩果酸、迷迭香酸、木犀草素、异鼠李素、山柰酚6个活性成分的含量,用以控制香青兰药材的质量。方法:样品经50%甲醇超声提取后,采用Thermo^TM UPLC-MS/MS仪、Waters^TM UPLC BEH C18色谱柱(2.1mm×100 mm,1.7μm)进行检测,并以0.1%甲酸水溶液(A)-乙腈(B)为流动相,梯度洗脱(0~2 min,95%A;2~8 min,95%A→5%A;8~10 min,5%A;10~10.1 min,5%A→95%A;10.1~12 min,95%A),流速0.3 mL·min-1,柱温30℃。正负离子切换扫描;喷雾电压:(+)3.2 kV、(-)3 kV;雾化温度:200℃;吹扫气压力:275.8 kPa;辅气压力:68.95 kPa;毛细管温度:350℃。结果:测定的6个化合物浓度在相应的范围(0.1838~11.2150 mg·L^-1)与峰面积呈良好的线性关系(R2=0.9992~0.9999);加样回收率(n=6)为91.4%~99.8%。不同批次香青兰中以苯丙素类化合物迷迭香酸的含量最高(6.00 mg·g-1),黄酮类成分山柰酚的含量最低(0.09 mg·g-1),产于新疆的香青兰药材质量较优。结论:该研究可用于香青兰中主要活性成分的含量测定,为该药材质量标准的完善提供参考。Objective:To establish an UPLC-MS/MS method for the determination of six contents(ursolic acid,oleanolic acid,rosemary acid,luteolin,isorhamnetin and kaempferol)in Dracocephalum moldavica L..Methods:The samples were extracted by 50%methanol.The chromatographic separation was performed on Thermo^TM UPLC-MS/MS,with an analytical column of Waters^TM UPLC BEH C18(2.1 mm×100 mm,1.7μm).Then 0.1%formic acid aqueous solution(A)and methanol(B)were used as the mobile phases for gradient elution(0-2 min,95%A;2-8 min,95%A→5%A;8-10 min,5%A;10-10.1 min,5%A→95%A;10.1-12 min,95%A).The flow rate was set at 0.3 mL·min-1 and the column temperature was 30℃.Positive and negative ion switching scanning;spray voltage:(+)3.2 kV,(-)3 kV;atomization temperature:200℃;purge gas pressure:275.8 kPa;auxiliary gas pressure:68.95 kPa;capillary temperature:350℃.Results:All the 6 flavonoids showed good linear relationship(R2=0.9992-0.9999)with the peak area within their tested ranges(0.1838-11.2150 mg·L^-1).The average recoveries of 6 flavonoids(n=6)were 91.4%-99.8%.Among the different batches of Dracocephalum moldavica L.,the content of phenylalanin compound rosemary acid was the highest(6.00 mg·g^-1),and the content of flavonoid kaempferol was the lowest(0.09 mg·g^-1).The quality of Dracocephalum moldavica L.from Xinjiang was superior.Conclusion:This study can be used to determine the active ingredients in Dracocephalum moldavica L.,and provide reference for the improvement of the quality standards of this herb.

关 键 词：超高效液相色谱串联-三重四极杆质谱 香青兰 活性成分 熊果酸 齐墩果酸 迷迭香酸 木犀草素 异鼠李素 山柰酚 含量测定 质量控制 

分 类 号：R917[医药卫生—药物分析学]