摘要
该文拟建立超高效液相色谱-三重四极杆-线性离子阱质谱(UHPLC-QTRAP-MS)方法同时测定半枝莲多指标成分的含量,为寻找半枝莲差异性质量控制成分提供参考。采用Thermo Acclaim^(TM) RSLC 120 C_(18)色谱柱(3.0 mm×100 mm,2.2μm),柱温40℃,进样量2μL,流动相A为0.1%甲酸水,流动相B为乙腈,流速0.4 mL·min^(-1),梯度洗脱,以多反应监测(MRM)方法进行质谱检测,利用聚类分析(HCA)及偏最小二乘法判别分析(PLS-DA)对数据进行处理。16个待测化合物在各自线性范围内均具有良好的线性关系,相关系数(R^(2))均大于0.9932,精密度、稳定性、重复性试验RSD≤3.7%,平均加样回收率在95.67%~104.8%,RSD≤3.2%,经HCA及PLS-DA,样品被聚集为4类,并通过变量权重重要性排序(VIP)发现野黄芩素、野黄芩苷、毛蕊花糖苷、半枝莲碱X为4类样品间的主要差异成分。结果表明所建立的方法可用于半枝莲中主要活性成分的同时测定及质量控制研究。
The present study developed an ultra-fast liquid chromatography coupled with triple quadrupole-linear ion trap composite mass spectrometry(UHPLC-QTRAP-MS)to simultaneously determine the content of potential active components in Scutellariae Barbatae Herba and also to provide a reference approach for screening out the differential quality control components among different batches of Scutellariae Barbatae Herba.Chromatographic separations were conducted on a Thermo Acclaim^(TM )RSLC 120 C_(18) column(3.0 mm×100 mm,2.2μm)in a gradient program.The mobile phase consisted of 0.1%aqueous formic acid and acetonitrile,and the column temperature was maintained at 40℃.The flow rate was 0.4 mL·min^(-1) and the injection volume was 2μL.The targeted compounds were monitored in the multiple reaction monitoring(MRM)mode.The acquired data were processed by hierarchical cluster analysis(HCA)and partial least square discriminant analysis(PLS-DA).Sixteen compounds all showed good linear relationship within the corresponding linear ranges and the R^(2) values were all higher than 0.9932.The RSDs of precision,repeatability,and stability were less than or equal to 3.7%.Mean recovery rates were in the range of 95.67%and 104.8%with RSDs≤3.2%.According to HCA and PLS-DA,all samples were clustered into four categories.Scutellarin,acteoside,scutellarein,and scutebarbatine X(VIP>1)were considered as differential chemical markers in the four categories.In conclusion,the developed method can be used for the simulta-neous determination of the multiple components and quality control of Scutellariae Barbatae Herba.
作者
蒋家璐
康安
李琴
宋蒙蒙
韩慧发
蔡雨晴
徐坠成
程海波
孙东东
JIANG Jia-lu;KANG An;LI Qin;SONG Meng-meng;HAN Hui-fa;CAI Yu-qing;XU Zhui-cheng;CHENG Hai-bo;SUN Dong-dong(School of Pharmacy,Nanjing University of Chinese Medicine,Nanjing 210023,China;Collaborative Innovation Center of Jiangsu Province of Cancer Prevention and Treatment of Chinese Medicine,Nanjing 210023,China;School of Integrated Chinese and Western Medicine,Nanjing University of Chinese Medicine,Nanjing 210023,China)
出处
《中国中药杂志》
CAS
CSCD
北大核心
2022年第2期437-443,共7页
China Journal of Chinese Materia Medica
基金
国家重点研发计划项目(2017YFC1700602)
国家自然科学基金项目(82074318,81930117,81973523)
江苏省自然科学基金项目(BK20171491)
江苏省中医药管理局科研项目(YB201809)。
