HPLC法测定含黄芪中药制剂中毛蕊异黄酮葡萄糖苷的含量  

Content Determination of Calycosin Glycoside in TCM Preparation Containing Astragalus membranaceus by HPLC Method

作　　者：陈莉[1] 王盛[1] 孟楣[1] CHEN Li;WANG Sheng;MENG Mei(Dept.of Pharmacy,the First Affiliated Hospital of Anhui University of TCM/Third Level Lab of TCM Preparation,State Administration of TCM,Hefei 230031,China)

机构地区：[1]安徽中医药大学第一附属医院药学部/国家中医药管理局中药制剂三级实验室,合肥230031

出　　处：《中国药房》2018年第15期2041-2045,共5页China Pharmacy

基　　金：国家科技支撑计划新安医学传承与发展研究项目(No.2012BAI26B03)

摘　　要：目的:建立一种测定含黄芪中药制剂中毛蕊异黄酮葡萄糖苷含量的方法。方法:以我院中药制剂养肝益水颗粒为模型药物,参照2015年版《中国药典》(一部)(简称"药典")中"黄芪"项下毛蕊异黄酮葡萄糖苷高效液相色谱(HPLC)含量测定方法,采用药典色谱条件并在此基础上,通过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,建立含黄芪中药制剂中毛蕊异黄酮葡萄糖苷含量测定方法,并进行方法学考察。然后用另外2种含黄芪的中药制剂对该法进行初步验证。结果:在药典色谱条件下,模型药物中的毛蕊异黄酮葡萄糖苷色谱峰不能与基线分离;优化后,得到流动相为乙腈-0.2%甲酸溶液(14∶86,V/V),检测波长为260 nm,柱温为30℃,流速为1.0 m L/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5.08~81.28μg/m L;精密度、稳定性、重复性试验的RSD均<2.0%(n=6);平均加样回收率为100.22%(RSD=0.95%,n=6)。经该法测定的5批模型药物中毛蕊异黄酮葡萄糖苷的平均含量为0.014 2%。经验证,该法也可有效分离另外2种含黄芪中药制剂中的毛蕊异黄酮葡萄糖苷。结论:成功建立测定含黄芪中药制剂中毛蕊异黄酮葡萄糖苷含量的HPLC法,且该法准确可靠,重现性好,具有一定适用性,可为后续深入研究奠定基础。OBJECTIVE:To establish a method for the content determination of calycosin glycoside in TCM preparation containing Astragalus membranaceus.METHODS:Using TCM preparation Yanggan yishui granules as model drug in our hospital,referring to HPLC method for content determination of calycosin glycoside stated in terms of“A.membranaceus”of 2015 edition of Chinese Pharmacopoeia(partⅠ)(called“pharmacopoeia”for short),use pharmacopoeia chromatogram condition and on this foundation to optimize and improve which by the method of increasing the formic acid proportion of mobile phase and prolonging the gradient elution time of the high polar segment of the mobile phase;the method was established for content determination of calycosin glycoside in TCM preparation containing A.membranaceus.Preliminary verification was carried out by using other two kinds of TCM preparation containing A.membranaceus.RESULTS:Under the chromatographic condition of pharmacopoeia,chromatographic peaks of calycosin glycoside in model drug could not be separated from the baseline.Optimized chromatographic condition included that mobile phase was acetonitrile-0.2%formic acid solution(14∶86,V/V);the detection wavelength was 260 nm;the column temperature was set at 30℃;the flow rate was 1.0 mL/min.Under optimal conditions,the linear range of calycosin glycoside was 5.08-81.28μg/mL.RSDs of precision,stability and reproducibility tests were all lower than 2.0%(n=6).Average recovery was 100.22%(RSD=0.95%,n=6).Average content of calycosin glycoside in 5 batches of model drugs by this method was 0.014 2%.After validation,the method could effectively isolate calycosin glycoside from other 2 kinds of TCM preparations containing A.membranaceus.CONCLUSIONS:Established HPLC method can be used for content determination of calycosin glycoside in TCM preparations containing A.membranaceus.The method is accurate,reliable,reproducible and suitable,which lays the foundation for further research.

关 键 词：含黄芪中药制剂 毛蕊异黄酮葡萄糖苷 高效液相色谱法 含量测定 

分 类 号：R284[医药卫生—中药学] R921[医药卫生—中医学]