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—Micro2000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AcquityUPLCBEHC18色谱柱(50mm×2.1mm,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0.3mL/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12.63—1616ng/mL(r=0.9998),12.44—1592ng/mL(r=0.9999),12.53。1604ng/mL(r=0.9994),12.94~1606ng/mL(r=0.9997),2.5—160ng/mL(r=0.9998)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。
AIM To establish a UPLC-MS method for simultaneous determining the contents of paeoniflorin, albiflorin, astragaloside IV, scutellarin and wogonin in Zengmian Yiliu Granules (Astragali Radix, Codonopsis Ra- dix, Paeoniae Radix alba, etc. ). METHODS UPLC-MS analyses were carried out on an Acquity UPLC BEH Cls column (50 mm ×2. 1 mm, 1.7μm, Waters, USA) with a mixture of 0. 1% formic acid aqueous containing 5 mmol ammonium acetate (A) and acetonitrile (B) as the mobile phase in a gradient mode. The flow rate was 0.3 mL/min and the column temperature was maintained at 30%. RESULTS The calibration curves of paeoniflorin, albiflorin, astragaloside IV, scutellarin and wogonin were in good linearity over the ranges of 12.63 - 1 616 ng/mL (r=0.999 8), 12. 44~1 592 ng/mL (r=0.999 9), 12.53-1 604 ng/mL (r=0.9994), 12.94~1 606 ng/mL ( r = 0. 999 7 ), 2. 5 - 160 ng/mL ( r = 0. 999 8 ), respectively, and the average recoveries were 101.6% (RSD=2.40%), 98.84% (RSD=2.75%), 97.89% (RSD=l.49%), 98.34% (RSD=2.03%), 97. 13% ( RSD = 1.73% ) , respectively. CONCLUSION The method is simple, feasible, and reproducible, and can be used for the quality control of Zengmian Yiliu Granules.