UPLC-MS法同时测定增免抑瘤颗粒中5种成分

目的建立同时测定增免抑瘤颗粒(黄芪、党参、白芍等)中芍药苷、芍药内酯苷、黄芪甲苷、野黄芩苷和汉黄芩素的UPLC-MS方法。方法采用Waters公司UPLC-Micro 2000仪器ESI+离子模式下选择离子监控,以柳胺酚为内标;色谱分离采用Acquity UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7μm);流动相为0.1%甲酸水溶液(含5mmol/L的乙酸铵)(A)-乙腈(B),梯度洗脱;体积流量0.3 mL/min;柱温30℃。结果芍药苷、芍药内酯苷、黄芪甲苷、野黄芩苷、汉黄芩素分别在12.63¹ 616 ng/mL(r=0.999 8),12.441 616 ng/mL(r=0.999 8),12.44¹ 592 ng/mL(r=0.999 9),12.531 592 ng/mL(r=0.999 9),12.53¹ 604 ng/mL(r=0.999 4),12.941 604 ng/mL(r=0.999 4),12.94¹60 6 ng/mL(r=0.999 7),2.5160 6 ng/mL(r=0.999 7),2.5¹60 ng/mL(r=0.999 8)范围内线性关系良好。平均回收率分别为101.6%(RSD为2.40%),98.84%(RSD为2.75%),97.89%(RSD为1.49%),98.34%(RSD为2.03%)和97.13%(RSD为1.73%)。结论所建立UPLC-MS方法简捷、准确、重复性好,可用于增免抑瘤颗粒剂的质量控制。

Simultaneous determination of five active constituents in Zengmian Yiliu Granules by UPLC-MS