HPLC波长切换法同时测定血脂灵片中7种成分的含量  

Simultaneous Determination of Seven Components in Xuezhiling Tablets(血脂灵片)by HPLC Wavelength Switching Method

作　　者：王艳萍 李宏 李鹏 Wang Yan-ping;LI Hong;LI Peng(Shangluo Drug Inspection Center,Shangluo Shaanxi 726000,China)

机构地区：[1]商洛市药品检验所,陕西商洛726000

出　　处：《中医药导报》2022年第2期48-52,共5页Guiding Journal of Traditional Chinese Medicine and Pharmacy

基　　金：陕西省中医药管理局科研项目(2019-GJ-LC022)。

摘　　要：目的:建立血脂灵片中23-乙酰泽泻醇B、23-乙酰泽泻醇C、橙黄决明素、芦荟大黄素、大黄素、大黄酚和大黄素甲醚7种成分的含量测定方法,为血脂灵片的质量评价提供实验参考。方法:采用HPLC波长切换法同时测定血脂灵片中23-乙酰泽泻醇B、23-乙酰泽泻醇C、橙黄决明素、芦荟大黄素、大黄素、大黄酚和大黄素甲醚7种化学成分的含量,色谱柱为Waters XBridge^(TM) C_(18)柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.1%磷酸水溶液,梯度洗脱;柱温为30℃,进样量为10μL;检测波长分别为λ1=208 nm、λ2=246 nm、λ3=284 nm。结果:23-乙酰泽泻醇B、23-乙酰泽泻醇C、橙黄决明素、芦荟大黄素、大黄素、大黄酚和大黄素甲醚分离度良好;分别在0.755~15.090μg/mL(r=0.9998)、0.765~15.390μg/mL(r=0.9999)、1.269~25.370μg/mL(r=0.9998)、1.268~25.360μg/mL(r=0.9999)、1.465~29.300μg/mL(r=0.9997)、1.240~24.800μg/mL(r=0.9998)、1.038~20.760μg/mL(r=0.9999)的范围内线性关系良好;平均回收率分别为99.98%(RSD=0.86%)、101.29%(RSD=0.92%)、100.88%(RSD=1.10%)、99.98%(RSD=0.92%)、101.50%(RSD=1.63%)、100.19%(RSD=0.55%)、99.95%(RSD=0.60%)(n=9)。结论:本研究同时定量分析了血脂灵片中7种指标性成分的含量,该法操作准确、重复性好,可客观、全面地对血脂灵片的内在质量进行有效评价。Objective:To establish a method for the determination of 23-acetyl alisol B,23-acetyl alisol C,aurantio obtusin,aloeemodin,emodin,chrysophanic acid and emodin methyl ether in Xuezhiling tablets,and to provide an experimental reference for the internal quality control of Xuezhiling tablets.Methods:The contents of 23-acetyl alisol B,23-acetyl alisol C,aurantio obtusin,aloeemodin,emodin,chrysophanic acid and emodin methyl ether in Xuezhiling tablets were detected by HPLC wavelength switching method.The chromatographic column was waters XBridge^(TM) C_(18) column(4.6 mm×250 mm,5μm).The mobile phase was acetonitrile-0.1%phosphoric acid in a gradient elution manner,the temperature of column was 30℃,the injection volume is 10μL,and detection wavelength was set atλ1=208 nm,λ2=246 nm,λ3=284 nm.Results:The separation of 23 acetylalisol B,23 acetylalisol C,orange cassia,aloe emodin,emodin,chrysophanol and emodin methyl ether was good.The linear relationship was good in the range of 0.755~15.090μg/mL(r=0.9998),0.765~15.390μg/mL(r=0.9999),1.269~25.370μg/mL(r=0.9998),1.268~25.360μg/mL(r=0.9999),1.465~29.300μg/mL(r=0.9997),1.240~24.800μg/mL(r=0.9998),and 1.038~20.760μg/mL(r=0.9999).And the average recoveries were 99.98%(RSD=0.86%),101.29%(RSD=0.92%),100.88%(RSD=1.10%),99.98%(RSD=0.92%),101.50%(RSD=1.63%),100.19%(RSD=0.55%),99.95%(RSD=0.60%)(n=9),respectively.Conclusion:The content of seven components were quantitatively analyzed in this study,and the operation of this method was accurate and reproducible,which could objectively and comprehensively evaluate the internal quality of Xuezhiling tablets.

关 键 词：血脂灵片 HPLC波长切换法 23-乙酰泽泻醇B 23-乙酰泽泻醇C 橙黄决明素 芦荟大黄素 大黄素 大黄酚 大黄素甲醚 含量测定 

分 类 号：R284.1[医药卫生—中药学]