跌打丸多指标含量测定方法研究及整体质量评价

Multi-component Quantification Analysis and Overall Quality Evaluation of Dieda Pills

目的建立HPLC-波长切换法同时测定跌打丸中芍药苷、柚皮苷、橙皮苷、新橙皮苷、丹皮酚、川续断皂苷Ⅵ、甘草酸、姜黄素和11-羰基-β-乙酰乳香酸的含量,用于评价跌打丸的整体质量。方法采用Agilent Poroshell 120 EC-C18(4.6 mm×100 mm,2.7μm)色谱柱,乙腈-0.1%磷酸溶液为流动相,梯度洗脱,检测波长:芍药苷为230 nm、柚皮苷、橙皮苷、新橙皮苷为283 nm,丹皮酚为274 nm,川续断皂苷Ⅵ为212 nm,甘草酸为251 nm,姜黄素为440 nm,11-羰基-β-乙酰乳香酸为251 nm。结果9种成分均能实现良好分离,其他成分无干扰。芍药苷、柚皮苷、新橙皮苷、11-羰基-β-乙酰乳香酸在0.1~1.0μg,橙皮苷、川续断皂苷Ⅵ在0.2~2.0μg,丹皮酚在0.04~0.4μg,甘草酸在0.02~0.2μg,姜黄素在0.01~0.1μg内呈良好的线性关系,相关系数均大于0.9998,平均回收率(n=6)均大于96.95%(RSD均小于0.86%)。结论该方法操作简便、选择性强、灵敏度和准确度高,可快速、有效的实现跌打丸的整体质量评价。

OBJECTIVE To establish an HPLC method for simultaneous determination of nine components,i.e.,paeoniflorin,naringin,hesperidin,neohesperidin,paeonol,asperosaponinⅥ,glycyrrhizic acid,curcumin and acetyl-11-keto-beta-boswellic acid,and evaluate the overall quality of Dieda pills.METHODS The analysis was performed on an Agilent 1260 Infinity LC System with a diode array detector.The chromatographic separation was performed on Agilent Poroshell 120 EC-C18(4.6 mm×100 mm,2.7μm)column.The mobile phase was a mixture of acetonitrile(mobile phase A)and water containing 0.1%phosphoric acid aqueous solution(mobile phase B).The gradient elution program was as follows:5%-18%A for 0-7 min,keeping 18%A for 7-15 min,18%-35%A for 15-27 min,35%-60%A for 27-32 min,60%-95%A for 32-42 min,keeping 95%A for 42-45 min.The flow rate was set at 1.0 mL·min-1,the column temperature was maintained at 30℃and the injection volume was 5μL.The detection wavelength was set at 230 nm for paeoniflorin,283 nm for naringin,hesperidin and neohesperidin,274 nm for paeonol,212 nm for asperosaponinⅥ,251 nm for glycyrrhizic acid,440 nm for curcumin and 251 nm for acetyl-11-keto-beta-boswellic acid,respectively.RESULTS All the nine components achieved good separation.The linear ranges fell with in the range of 0.1-1.0μg for paeoniflorin,naringin,neohesperidin andacetyl-11-keto-beta-boswellic acid,0.2-2.0μg for hesperidin and asperosaponinⅥ,0.04-0.4μg for paeonol,0.02-0.2μg for glycyrrhizic acid and 0.01-0.1μg for curcumin,respectively(r^2≥0.9998).The average recoveries(n=6)were 96.95%-100.4%and the RSDs were 0.21%-0.81%.CONCLUSION The developed method is simple,accurate,reliable,and can be used for the overall quality control and quality evaluation of Dieda pills.