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HPLC-ELSD测定心脑舒通胶囊中Terrestrinin A的含量
张娜1,2, 栾晓莹1, 谢燕1,2, 柏自松1,2, 白洋1, 胡利民1, 常艳旭1, 王萌1, 张鹏1
1.天津中医药大学, 天津市现代中药重点实验室, 天津 300193;2.天津国际生物医药联合研究院, 中药新药研发中心, 天津 300457
摘要:
[目的] 建立心脑舒通胶囊及其总皂苷中Terrestrinin A含量的测定方法。[方法] 采用高效液相色谱-蒸发光散射检测器(HPLC-ELSD)法,色谱柱为Hedra-C18柱(4.6 mm×150 mm,5 μm),流动相:乙腈-水,流速:1 mL/min,柱温:40℃,漂移管温度:60℃,气体(N2)压力:30 psi,增益值:100,进样量:20 μL。[结果] 线性范围:48.5~970.6 μg/mL,回归方程:Ŷ =1.6931X+1.2644(r2≥0.9990),精密度、重复性和稳定性实验的RSD值分别是1.21%、1.62%、1.90%,加样回收率是96.0%~103.2%,RSD值是2.40%。[结论] 该法简便可靠,可以应用于心脑舒通胶囊及其总皂苷中Terrestrinin A的含量测定及质量控制标准建立。
关键词:  心脑舒通胶囊  蒺藜  Terrestrinin A  HPLC-ELSD  含量测定
DOI:10.11656/j.issn.1673-9043.2017.02.14
分类号:
基金项目:重大新药创制项目(2011ZX09201-201);国家自然科学基金青年项目(81303183)
Determination of Terrestrinin A from Xinnao Shutong capsules by HPLC-ELSD method
ZHANG Na1,2, LUAN Xiao-ying1, XIE Yan1,2, BAI Zi-song1,2, BAI Yang1, HU Li-min1, CHANG Yan-xu1, WANG Meng1, ZHANG Peng1
1.Tianjin University of Traditional Chinese Medicine, Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin 300193, China;2.Tianjin International Joint Academy of Biomedicine, Research and Development Center of Traditional Chinese Drug, Tianjin 300457, China
Abstract:
[Objective] To establish a quantitative method for the determination of Terrestrinin A in Xinnao Shutong capsules and total saponins. [Methods] Using HPLC ELSD method, chromatography column Hedra-C18 column (4.6 mm×150 mm, 5 microns), mobile phase:acetonitrile-water, flow rate:1 mL/min, column temperature:40℃, drift tube temperature:60℃, gas pressure (N2):30 psi, gain:100, sample quantity:20 μL. [Results] Linear range:48.5 to 970.6 μg/mL, the regression equation:Ŷ=1.693 1+1.264 4X (r2=0.9990), precision, repeatability and stability testing of RSD value was 1.21%, 1.62%, 1.9% respectively, the recovery rate is 96.0%-103.2%, RSD value was 2.4%. [Conclusion] The method is simple and reliable, and can be applied to determine the content of Terrestrinin A in Xinnao Shutong capsule and total saponins preserving method and establish quality control standards.
Key words:  Xinnao Shutong capsules  Tribulus terrestris L.  Terrestrinin A  HPLC-ELSD  quantitative determination
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