摘要
目的:建立一测多评(QAMS)法测定小儿豉翘清热颗粒中栀子苷、芍药苷、连翘酯苷A、黄芩苷、连翘苷、千层纸素A-7-O-β-D-葡萄糖醛酸苷、汉黄芩苷、黄芩素、汉黄芩素9个成分的含量。方法:采用超高效液相色谱法,Acquity UPLC BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm);乙腈(A)-0.2%磷酸水溶液为流动相(B),梯度洗脱;流速0.25 mL·min^(-1),柱温25℃,检测波长220 nm。以黄芩苷为内参物,建立栀子苷、芍药苷、连翘酯苷A、连翘苷、千层纸素A-7-O-β-D-葡萄糖醛酸苷、汉黄芩苷、黄芩素、汉黄芩素与内参物黄芩苷的相对校正因子(f),通过f计算小儿豉翘清热颗粒中9个成分的含量,并进行验证,将该方法与外标法(ESM)的测定结果进行对比分析,以验证QAMS方法的准确性、重复性及可行性。结果:栀子苷、芍药苷、连翘酯苷A、黄芩苷、连翘苷、千层纸素A-7-O-β-D-葡萄糖醛苷、汉黄芩苷、黄芩素、汉黄芩素的质量浓度分别在9.953～199.1μg·mL^(-1)、5.994～119.9μg·mL^(-1)、4.390～87.80μg·mL^(-1)、9.819～196.4μg·mL^(-1)、1.802～36.04μg·mL^(-1)、1.408～28.17μg·mL^(-1)、2.551～51.02μg·mL^(-1)、0.140 2～2.804μg·mL^(-1)、0.361 3～7.225μg·m L^(-1)范围内线性关系良好;加样回收率在95.7%～102.5%;以黄芩苷为内参物,测得的f值分别为4.621 1、4.105 5、1.825 3、1.796 5、1.040 2、1.339 8、0.647 4、0.888 7,且建立的QAMS法计算结果与外标法(ESM)的计算结果之间无显著性差异。结论:本实验建立的QAMS法可作为一种简便快捷的质量评价模式,用于小儿豉翘清热颗粒中9个成分的质量控制。
Objective：To determine 9 components,including geniposide,paeoniflorin,forsythoside A,baicalin,forsythin,oroxylin A-7-O-glucuronide,wogonoside,baicalein and wogonin in Xiao＇er Chiqiao Qingre granules by multi-components with a single-marker（QAMS）method.Methods：The UPLC separation was achieved onan Acquity UPLC BEH C_（18） column（100 mm×2.1 mm,1.7 μm）with acetonitrile（A）-0.2% phosphoric acid solution（B）as mobile phase at a flow rate of 0.25 mL·min-1 with gradient elution.The column temperature was set at 25 ℃.The determination wavelength was 220 nm.With baicalin as the internal reference standard,the relativecorrection factors（f）of geniposide,paeoniflorin,forsythoside A,forsythin,oroxylin A-7-O-glucuronide,wogonoside,baicalein and wogonin were calculated.The method was evaluated by comparison of the quantitative results between external standard method（ESM） and QAMS.Results：Geniposide、paeoniflorin、forsythoside A、baicalin、forsythin、oroxylin A-7-O-glucuronid、wogonoside、baicalein and wogonin had good relations within the range of 9.953-199.1 μg·m L-1,5.994-119.9μg·m L-1,4.390-87.80 μg·m L-1,9.819-1）96.4 μg·m L-1,1.802-36.04 μg·m L-1,1.408-28.17 μg·m L^（-1,2.551-51.02 μg·m L-1,0.140 2-2.804 μg·m L-1 and 0.361 3-7.225 μg·mL-1,respectivley.The recoveries were within 95.7% and 102.5%.With baicalin as the internal reference standard,the relative correction factors（f）were 4.621 1,4.105 5,1.825 3,1.796 5,1.040 2,1.339 8,0.647 4 and 0.888 7, respectively.No significant difference was observed between the results of two methods.Conclusion：The QAMS method is simple and fast,and can be used to determine the multiple components in Xiao＇er Chiqiao Qingre granules.
作者
田刚
李超
吴菲
刘雪
杨学芳
姚令文
TIAN Gang;LI Chao;WU Fei;LIU Xue;YANG Xue-fang;YAO Ling-wen(Jumpcan Pharmaceutical Co.,Ltd.,Taizhou 225411,China;National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第11期1922-1930,共9页
Chinese Journal of Pharmaceutical Analysis
基金
国家医药管理局标准化建设项目(ZYBZH-C-JS-33)
