摘要
目的:建立UPLC-MS/MS同时测定红五参胶囊中11个成分(咖啡酸、阿福豆苷、没食子酸、新绿原酸、绿原酸、隐绿原酸、红景天苷、紫丁香苷、人参皂苷Re、人参皂苷Rg1、人参皂苷Rd)含量的方法.方法:采用Shim-pack GIST C18(100 mm ×2.1 mm,2 μm)色谱柱,以乙腈-0.1％乙酸-1 mmol·L-1 乙酸铵水溶液为流动相,梯度洗脱,流速0.3 mL·min-1,柱温30℃,进样量为1 μL;采用电喷雾电离源(ESI源),多反应监测(MRM)模式进行正负离子检测.结果:11个成分在测定浓度范围内线性关系良好,线性相关系数r均＞0.999 0;精密度RSD均＜3％;重复性和稳定性良好,RSD值均＜5％;平均加样回收率为97.1％～101.5％,RSD≤3.7％.10批红五参胶囊中咖啡酸、阿福豆苷、没食子酸、新绿原酸、绿原酸、隐绿原酸、红景天苷、紫丁香苷、人参皂苷Re、人参皂苷Rg1、人参皂苷Rd含量分别为0.010～0.013、0.000 7～0.001 4、0.035～0.038、0.312～0.315、0.413～0.417、0.411～0.416、4.355～4.358、0.030～0.032、0.993～0.999、1.120～1.124、2.536～2.538 mg·g-1.结论:本方法准确灵敏,稳定性和重复性良好,可用于红五参胶囊的质量控制.
Abstract
Objective:To establish an UPLC-MS/MS method for simultaneous determination of 11 components(caffeic acid,afzelin,gallic acid,neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,salidroside,eleuth-eroside B,ginsenoside Re,ginsenoside Rg1,ginsenoside Rd)in Hongwushen capsules.Methods:A Shim-pack GIST C18 chromatographic column(100 mm ×2.1 mm,2 μm)was used.The mobile phase was composed of ace-tonitrile-0.1％acetic acid-1 mmol·L-1 ammonium acetate aqueous solution and the gradient elution was ap-plied.The flow rate was 0.3 mL·min-1,the column temperature was 30 ℃,and the injection volume was 1μL.Electrospray ionization(ESI)source and multiple reaction monitoring(MRM)mode in both positive and negative were used for ion detections.Results:The linear relationship of 11 components was good in the concen-tration range,and the linear correlation coefficients were all above 0.999 0.The RSD values of precision were less than 3％.The repeatability and stability were good,and the RSD values were less than 5％.The average recover-ies were in the range of 97.1％-101.5％with RSDs≤3.7％.The contents of caffeic acid,afzelin,gallic acid,neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,salidroside,eleutheroside B,ginsenoside Re,gin-senoside Rg1 and ginsenoside Rd in 10 batches of Hongwushen capsules were 0.010-0.013 mg·g-1,0.000 7-0.001 4 mg·g-1,0.035-0.038 mg·g-1,0.312-0.315 mg·g-1,0.413-0.417 mg·g-1,0.411-0.416 mg·g-1,4.355-4.358 mg·g-1,0.030-0.032 mg·g-1,0.993-0.999 mg·g-1,1.120-1.124 mg·g-1 and 2.536-2.538 mg·g-1,respectively.Conclusions:The method is accurate,sensitive,stable and reproduci-ble,and can be used for the quality control of Hongwushen capsules.
基金项目
河北省省级科技计划(23372502D)
河北省自然科学基金(H2022423341)
河北省自然科学基金(H2022423335)
国家级大学生创新创业训练计划(202214432020)
河北中医药局项目(2022107)
NETL
NSTL
万方数据