摘要
目的:建立扶阳通便颗粒质量标准。方法:采用薄层色谱法(TLC)对扶阳通便颗粒干姜中的6-姜辣素进行定性鉴别,并对黑顺片中的双酯型生物碱进行限量检查;采用高效液相色谱法(HPLC)对肉苁蓉中的松果菊苷含量进行测定。色谱柱为GL Sciences C_(18)柱(4.6 mm×250 mm,5μm),流动相为甲醇(A)-0.1%甲酸溶液(B),梯度洗脱程序:0~17 min,26.5%A;17~20 min,26.5%A→29.5%A;20~56 min,26.5%A。流速为1.0 mL/min,检测波长为330 nm,柱温40℃,进样量10μL。结果:干姜中6-姜辣素和黑顺片中乌头类双酯型生物碱的TLC图斑点清晰且分离度较好,阴性对照无干扰。建立了松果菊苷的HPLC含量测定方法,松果菊苷浓度在12.51~200.10μg/mL(r=0.999 97)范围内具有良好的线性关系,精密度、稳定性(24 h)、重复性试验的RSD均<2%,平均回收率为99.7%,RSD为1.44%(n=6)。结论:本研究所建立的鉴别、限量检查及含量测定方法准确可靠,可为扶阳通便颗粒的质量控制提供科学依据。
Objective:To establish the quality standard of Fuyang Tongbian Granules.Methods:Thin layer chromatography(TLC)was used for the qualitative identification of 6-gingerol in Zingiberis Rhizoma and the limit test of diester-type aconite alkaloids in Aconiti Lateralis Radix Praeparata.The content of echinacoside in Cistanches Herba was determined by high performance liquid chromatography(HPLC).The chromatography was performed on GL Sciences C_(18) column(4.6 mm×250 mm,5μm)with mobile phase consisting of methanol(A)-0.1%formic acid solution(B).The gradient elution procedure was 0~17 min,26.5%A;17-20 min,26.5%A→29.5%A;20~56 min,26.5%A.The flow rate was 1.0 mL/min,the detection wavelength was 330 nm,the column temperature was 40℃,and the sample size was 10μL.Results:The TLC spots of 6-gingerol and diester alkaloids were clear,with good separation and without negative interference.The content determination method of echinacoside by HPLC was established.The linear range of echinacoside was 12.51~200.1μg/mL(r=0.99997),and the RSD of precision,stability(24 h),and repeatability test results were all lower than 2.0%.The average sample recovery rate was 99.07%(RSD=1.44%,n=6).Conclusion:The identification,limit test and content determination methods are accurate and reliable,which can provide scientific reference for the quality control of Fuyang Tongbian Granules.
作者
曹昌娥
杨靖
邓祎
王琪
吴礼龙
鲍云惠
黄蕾
吕锁忠
吴安飞
CAO Chang'e;YANG Jing;DENG Yi;WANG Qi;WU Lilong;BAO Yunhui;HUANG Lei;LYU Suozhong;Wu Anfei(Qujing Hospital of Traditional Chinese Medicine,Qujing 65500,Yunnan,China)
出处
《上海中医药大学学报》
2025年第S1期100-106,共7页
Academic Journal of Shanghai University of Traditional Chinese Medicine
基金
云南省应用基础研究-中医联合面上项目(2017FF117-053)
关键词
扶阳通便颗粒
干姜
肉苁蓉
乌头类双酯型生物碱
质量标准
高效液相色谱法
薄层色谱法
Fuyang Tongbian Granules
Zingiberis Rhizoma
Cistanches Herba
diester-type aconite alkaloids
quality standard
high performance liquid chromatography
thin layer chromatography
