摘要
目的 建立同时测定珍龙醒脑胶囊中没食子酸、肉桂酸、甘草苷、西红花苷I、西红花苷II、桂皮醛、丁香酚、甘草次酸、麝香酮等9种成分的UPLC-DAD方法。方法 采用RP-UPLC法,Agilent Zorbax C18色谱柱（100 mm×2.1 mm,1.8μm）,流动相为0.1%甲酸水溶液-乙腈,体积流量0.3 m L/min,梯度洗脱,柱温35℃,进样量为1μL。分别对待测物考察其提取溶剂、线性范围、精密度、重复性、稳定性、加样回收率等方法学内容。结果 9种指标成分没食子酸在0.2-20.0mg/L（r=0.999 0）、西红花苷I在0.022-2.200 mg/L（r=0.999 3）、西红花苷II在0.02-2.00 mg/L（r=0.999 6）、甘草苷在0.093-1.860 mg/L（r=0.999 4）、肉桂酸在0.020 4-2.040 0 mg/L（r=0.999 9）、桂皮醛在0.042-4.200 mg/L（r=0.999 9）、丁香酚在0.95-95.00 mg/L（r=0.999 9）、甘草次酸在0.012 9-1.290 0 mg/L（r=0.998 9）、麝香酮在0.073 8-7.380 0 mg/L（r=0.999 0）线性关系良好;精密度RSD≤1.02%;重复性良好,RSD≤1.13%;加样回收率在93.8%-112.1%,RSD≤1.28%。供试品溶液在室温条件下24 h内稳定。3批次供试品中没食子酸、西红花苷I和II、甘草苷、肉桂酸、桂皮醛、丁香酚、甘草次酸、麝香酮质量分数分别为0.422-0.448、0.093-0.105、0.096-0.112、0.026 8-0.028 5、0.142-0.153、0.140-0.158、1.519-1.547、0.007 55-0.008 04、0.117-0.121 mg/g。结论 本法快速、灵敏度高、准确度高、专属性好,为珍龙醒脑胶囊的质量控制提供依据。
Objective To develop an UPLC-DAD method for simultaneous determination of gallic acid, cinnamic acid, licorice glycosides, crocin I, crocin II, cinnamic aldehyde, eugenol, glycyrrhetinic acid, and muscone in Zhenlong Xingnao Capsule. Methods Analysis was performed on a RP-UPLC method and an Agilent Zorbax C18 chromatographic column （100 mm × 2.1 ram, 1.8 μm） eluted with 0.1% formic acid （mobile phase A） and acetonitrile （mobile phase B）, the flow rate was 0.3 mL/min, gradient elution and column temperature was 35℃, the injection volume was 1 uL. Respectively to measure their extraction solvent, linear range, precision, repeatability, stability, and recovery rate. Results The nine components were well separated and showed good linearity, such as gallic acid 0.2-20.0 mg/L （r = 0.999 0）, crocin I 0.022-2.200 mg/L （r = 0.999 3）, crocin II 0.02-2.00 mg/L （r = 0.999 6）, licorice glycosides 0.093-1.860 mg,/L （r = 0.999 4）, cinnamic acid 0.020 4-2.040 0 mg/L （r = 0.999 9）, Cinnamic aldehyde 0.042- 4.200 mg/L （r = 0.999 9）, eugenol 0.95-95.00 mg/L （r = 0.999 9）, glycyrrhetinic acid 0.012 9-1.290 0 mg/L （r = 0.998 9）, and muscone 0.073 8-7.380 0 mg/L （r = 0.999 0）. The precision was good, RSD was 1.02% or less, The repeatability is good in terms of RSD of 1.13% or less and the recovery rate was 93.8%-112.1% （RSD 1.28% or less）. Test solution was stable at room temperature within 24 h. The contents of three batches of the gallic acid, crocin I, crocin II, licorice glycosides, cinnamic acid, cinnamic aldehyde, eugenol, glycyrrhetinic acid, and muscone were 0.422-0.448, 0.093-0.105, 0.096-0.112, 0.026 8-0.028 5, 0.142-0.153, 0.140-0.158, 1.519-1.547, 0.007 55-0.008 04, 0.117-0.121 rag/g, respectively. Conclusion The method is rapid and has high sensitivity, high accuracy, and good specificity, It can be applied to the quality control of Zhenlong Xingnao Capsule.
出处
《中草药》
CAS
CSCD
北大核心
2015年第13期1926-1930,共5页
Chinese Traditional and Herbal Drugs
基金
山东省中医药科技发展计划项目(2011-238)
