摘要
目的建立高效液相色谱(HPLC)法同时测定贯叶金丝桃及相关药品中金丝桃苷、金丝桃素含量的方法。方法采用Hypersil GOLDTM C18 LC色谱柱(150 mm×4.6 mm,5μm);流动相为乙腈-0.05%磷酸水溶液(pH 2.30~2.32)-乙酸铵缓冲液(0.15 mol·L^-1,pH 4.10~4.14),梯度洗脱(0~11 min,乙腈25%-0.05%磷酸水溶液75%;11~18 min,乙腈90%-乙酸铵缓冲液10%;18~22 min,乙腈25%-0.05%磷酸水溶液75%);流速1.0 mL·min^-1;检测波长360 nm和590 nm;柱温25℃;进样量10μL。按外标法定量分析。结果金丝桃苷和金丝桃素分别在0.8600~4.3000、0.0188~0.1500μg范围内与峰面积呈良好线性关系(r≥0.9996);其精密性、重复性、稳定性的相对标准偏差(RSD)均小于2%;平均加标回收率分别为98.33%(n=6)和99.20%(n=6)。结论该法快速、准确、分离度高,可用于贯叶金丝桃及相关药品中金丝桃苷和金丝桃素的含量测定。
Objective To develop a HPLC method for simultaneous determination of the contents of hyperoside and hypericin in Hypericum perforatum L.and related drugs.Methods The analysis was achieved with an Hypersil GOLDTM C18 LC column(150 mm×4.6 mm,5μm)with mobile phase consisted of acetonitrile-0.05%phosphoric acid(pH 2.30-2.32)-ammonium acetate buffer(0.15 mol·L^-1,pH 4.10-4.14),and the gradient elution system was performed as follows:0-11 min,25%acetonitrile,75%phosphoric acid;11-18 min,90%acetonitrile,10%ammonium acetate buffer;18-22 min,25%acetonitrile,75%phosphoric acid.The flow rate was 1.0 mL·min-1,the detection wavelengths were 360 nm and 590 nm,the column temperature was 25℃,the injection volume was 10μL.The external standard method was used in quantification.Results The linear ranges were 0.8600-4.3000μg for hyperoside and 0.0188-0.1500μg for hypericin,respectively(r≥0.9996).The RSDs of the precision,stability and reproducibility tests were all lower than 2%.The average recoveries of added standard were 98.33%and 99.20%(n=6),respectively.Conclusion The method is rapid,accurate,good with resolution,and can be used to determine the contents of hyperoside and hypericin simultaneously in Hypericum perforatum L.and related drugs.
作者
任晓霞
马君义
李茂星
吕孝飞
田秀玉
马生辉
陈丽萍
张继
REN Xiaoxia;MA Junyi;LI Maoxing;LYU Xiaofei;TIAN Xiuyu;MA Shenghui;CHEN Liping;ZHANG Ji(College of Life Science,Northwest Normal University,Lanzhou 730070 Gansu,China;Key Laboratory of the Prevention and Cure for the Plateau Environment Damage of PLA,Department of Pharmacy,The 940 Hospital of PLA Joint Logistics Support Forces,Lanzhou 730050 Gansu,China;College of Pharmacy,Lanzhou University,Lanzhou,Gansu 730030,China;Fuxiang Chinese Medicine Planting Farmers Professional Cooperative of Kangxian,Kangxian 746500 Gansu,China)
出处
《中药新药与临床药理》
CAS
CSCD
北大核心
2019年第11期1374-1378,共5页
Traditional Chinese Drug Research and Clinical Pharmacology