人参杞黄颗粒中毛蕊异黄酮葡萄糖苷的含量测定  

Content Determination of the Calycosin Glycoside in Renshen Qihuang Granules

作　　者：李素凯 刘露[1] 刘梦燕 李萍[1] 陈笑宇 李冬冬[1] 杨锦竹[1] 王伟 LI Su-kai;LIU Lu;LIU Meng-yan;LI Ping;CHEN Xiao-yu;LI Dong-dong;YANG Jin-zhu;WANG Wei(Jilin University,Changchun 130012,China;Institute for Food Inspection of Jilin Province,Changchun 130012,China)

机构地区：[1]吉林大学,吉林长春130012 [2]吉林省食品检验所,吉林长春130012

出　　处：《特产研究》2021年第4期90-94,共5页Special Wild Economic Animal and Plant Research

基　　金：吉林省科技厅科技服务计划项目“保健食品、生物健康材料产业化开发”(20200708062YY)。

摘　　要：本研究建立一种高效液相色谱(HPLC)方法测定人参杞黄颗粒中毛蕊异黄酮葡萄糖苷的含量。参照2020年版《中国药典》(一部)(简称"药典")中"黄苠"项下毛蕊异黄酮葡萄糖苷HPLC含量测定方法,根据药典并在此基础上,通过改善供试品处理方法,增加流动相甲酸比例、延长流动相大极性段洗脱时间等方法进行优化改进,建立了人参杞黄颗粒中毛蕊异黄酮葡萄糖苷含量测定方法,并进行方法学考察。结果显示,在药典色谱条件下,人参杞黄颗粒中的毛蕊异黄酮葡萄糖苷色谱峰与基线不能分:基于此将供试品通过D101型大孔吸附树酯柱进行洗脱,并对色谱条件进行优化最后得到以Amethyst C18-H柱(4.6mm×250mm,5μm)为色谱柱,以乙腈(A)~0.2%甲酸溶液(B)为流动相,梯度洗脱(0~50min,12%;50~80min,12%~50%A),检测波长为260nm,柱温为25℃,流速为1.0 mL/min的色谱条件。优化条件下毛蕊异黄酮葡萄糖苷质量浓度线性范围为0.004~0.024 mg/mL精密度、稳定性和重复性试验的RSD均<2.0%(n=6);平均加样回收率为99.26%(RSD=0.8143%,n=6)。从而得出结论:本研究成功建立了测定人参杞黄颗粒中毛蕊异黄酮葡萄糖苷含量的HPLC方法,该方法准确可靠,重现性好,在中药制剂方面具有一定适用性,可为其质量标准深入研究奠定基础。The study established a HPLC method for the content determination of calycosin glycoside in Renshen Qihuang Granules.Referring to the HPLC method for the content determination of calycosin glycoside stated in terms of A.membranaceus"of 2020 edition of Chinese Pharmacopoeia(partⅠ)(called"pharmacopoeia"for short),using pharmacopoeia chromatogram condition and on this foundation to improve the treatment method of test products,optimizing and improving the method of increasing the formic acid proportion of mobile phase and prolonging the gradient elution time of the high polar segments of the mobile phase;The method was established for the content determination of the calycosin glycoside in Renshen Qihuang Granules,and the methodological review was carried out.The results showed that under the chromatographic condition of pharmacopoeia,the chromatographic peaks of calycosin glycoside in Renshen Qihuang Granules could not be separated from the baseline.Based on this,the test products were eluted by D101 macroporous adsorbent resin column,and the chromatographic conditions were optimized.Finally,The Amethyst C18-H column(4.6 mm×250 mm,5μm)was used as the chromatographic column.Using acetonitrile(A)~0.2% formic acid solution(B)as the mobile phase,using the gradient elution(0~50 min,12%A;50~80 min,12%~50%A),the detection wavelength was 260 nm,the column temperature was 25℃,and the flow rate was 1.0 mL/min.The linear range of the mass concentration of the isoflavone glucoside was 0.004~0.024 mg/mL under the optimized conditions.RSDs of the precision,stability and reproducibility tests were all lower than 2.0%(n=6).The average recovery was 99.26%(RSD=0.8143%,n=6).Therefore,the HPLC method for the determination of Calycosin Glycoside in Renshen Qihuang Granules has been successfully established.The method is accurate,reliable and reproducible,and has certain applicability in the field of traditional Chinese medicine preparation,which could lay a foundation for the further study of quality standards.

关 键 词：毛蕊异黄酮葡萄糖苷 高效液相色谱法 含量测定 人参芪黄颗粒 

分 类 号：R284[医药卫生—中药学] O657.72[医药卫生—中医学]