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.
作者
陈洁
CHEN Jie(The Third People’s Hospital of Haikou,Haikou 571100,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2020年第11期1986-1993,共8页
Chinese Journal of Pharmaceutical Analysis
