一测多评法测定防风中6个有效成分的含量  

Simultaneous determination of six kinds of components in Saposhnikoviae Radix by QAMS

作　　者：张军鹏 庄辉 刘斌 周海燕 ZHANG Jun-peng;ZHUANG Hui;LIU Bin;ZHOU Hai-yan(Taian Testing Institute for Food and Drug Control,Taian 271000,China;Shandong Center for Food and Drug Evaluation&Inspection,Jinan 250000,China)

机构地区：[1]泰安市食品药品检验检测研究院,泰安271000 [2]山东省食品药品审评查验中心,济南250000

出　　处：《药物分析杂志》2023年第7期1163-1171,共9页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立测定防风中升麻素苷、升麻素、5-O-甲基维斯阿米醇苷、亥茅酚苷、补骨脂素、欧前胡素6个成分含量的一测多评方法,并验证该方法的准确性和可行性。方法:采用液相色谱法,应用Agilent ZORBAX SB-C18(250 mm×4.6 mm, 5μm)色谱柱,以乙腈(A)-0.02%的磷酸水溶液(B)为流动相,梯度洗脱,流速1.0 mL·min^(-1),柱温30℃,检测波长210 nm。以升麻素苷为内参物,分别建立升麻素、5-O-甲基维斯阿米醇苷、亥茅酚苷、补骨脂素、欧前胡素的相对校准因子,利用该相对校准因子计算其他5个成分含量,同时利用外标法测定各成分含量,比较2种测定方法的差异,验证一测多评法的可行性和适用性。结果:12批不同产地和批号的防风中6个有效成分采用一测多评法与外标法的实测值之间无显著性差异。12批防风中升麻素苷、升麻素、5-O-甲基维斯阿米醇苷、亥茅酚苷、补骨脂素、欧前胡素在测定范围内线性良好,含量范围分别为0.21%~0.49%、0.060%~0.16%、0.20%~0.41%、0.11%~0.26%、0.029%~0.093%、0.066%~0.14%。结论:一测多评法测定防风中升麻素苷、升麻素、5-O-甲基维斯阿米醇苷、亥茅酚苷、补骨脂素、欧前胡素6个成分准确可行,可用于防风的质量控制。Objective:To establish quantitative analysis of multi-components to a single-marker(QAMS)method for determining contents of six ingredients(prim-O-glucosylcimifugin,cimifugin,5-O-methylvisammioside,sec-O-glucosylhamaudol,psoralen and imperatorin)in Saposhnikoviae Radix and to verify the accuracy and feasibility of the method.Methods:A stable HPLC method was established and Agilent ZORBAX SB-Cis(250 mm×4.6 mm,5μm)column was adopted,the mobile phase consisted of acetonitrile(A)-0.02%phosphoric acid(B)in a gradient mode.The flow rate was 1.0 mL·min^(-1),the column temperature was set at 30℃,and the detection wavelength was set at 210 nm.QAMS method was established and validated for Saposhnikoviae Radix.Cimifugin,5-0-methylvisammioside,sec-O-glucosylhamaudol,psoralen and imperatorin were selected an analytes while prim-O-glucosylcimifugin was chosen as internal reference substance to evaluate the quality.The relative correction factors(RCFs)of prim-O-glucosylcimifugin to the other five active ingredients were calculated.The method was evaluated by the comparison of quantity between external standard method(ESM)and QAMS method.Results:The contents of six active ingredients in 12 batches of Saposhnikoviae Radix determined by QAMS method had no significantly different with external standard method.Prim-O-glucosylcimifugin,cimifugin,5-O-methylvisammioside,sec-O-glucosylhamaudol,psoralen,imperatorin showed good linear relationship in the ranges of 0.21%-0.49%,0.060%-0.16%,0.20%-0.41%,0.11%-0.26%,0.029%-0.093%,0.066%-0.14%,respectively.Conclusion:The determination results of prim-0-glucosylcimifugin,cimifugin,5-O-methylvisammioside,sec-O-glucosylhamaudol,psoralen and imperatorin in Saposhnikoviae Radix by QAMS is accurate and feasible,which can be used for the quality control of Saposhnikoviae Radix.

关 键 词：防风 一测多评 相对校正因子 升麻素苷 升麻素 5-O-甲基维斯阿米醇苷 亥茅酚苷 补骨脂素 欧前胡素 含量测定 

分 类 号：R917[医药卫生—药物分析学]