高效液相色谱测定除脂生发片中丹皮酚、黄柏酮、5-O-甲基维斯阿米醇苷和胡薄荷酮

Determination of paeonol,obacunone,5-O-methylvisamitol side and pulegone in Chuzhi Shengfa Tablets by high performance liquid chromatography

建立高效液相色谱波长切换法测定除脂生发片中丹皮酚、黄柏酮、5-O-甲基维斯阿米醇苷和胡薄荷酮成分含量。色谱柱为Agilent EclipsePlus C18(250 mm×4.6 mm,5μm);以乙腈(流动相A)-0.3%磷酸(流动相B)为流动相,梯度洗脱;柱温30℃;柱流量1.0 mL/min;丹皮酚、黄柏酮、5-O-甲基维斯阿米醇苷和胡薄荷酮的检测波长分别为274、236、254和252 nm;进样体积:10μL,高效液相色谱-二极管阵列检测器定量检测。丹皮酚、黄柏酮、5-O-甲基维斯阿米醇苷和胡薄荷酮分别在质量浓度0.01996~1.996、0.5868~5.868、0.997~9.97、0.0998~9.98μg/mL内与其色谱峰面积呈线性关系,相关系数分别为0.9996、0.9980、0.9997和0.9999,平均回收率分别为100.92%、100.54%、101.14%、100.93%;测定结果的相对标准偏差均小于5.0%(n=6)。该方法具有样品处理简单、分析时间短、检测结果准确等优点,适用于除脂生发片制剂的质量控制。

A high performance liquid chromatography wavelength switching method was established for the determination of paeonol,obacunone,5-O-methylvisammioside and pulegone in Chuzhi Shengfa Tablets.Agilent Eclipse Plus C18(250 mm×4.6 mm,5µm)was used.The mobile phase was consisted of acetonitrile(A)-0.3%phosphoric acid solution(B)with gradient elution.Column temperature was 30℃,column flow was 1.0 mL/min.Detection wavelengths of paeonol,xibutanone,5-O-methylvisamitol side and humenthone were set at 274,236,254 and 252 nm,respectively.Injection volume was 10µL.High performance liquid chromatography-diode array detector was used for quantitative detection.The mass fractions of paeonol,obacunone,5-O-methylvisamitol side and pulegone showed good linear relationships with their chromatographic peak area in range of 0.01996-1.996,0.5868-5.868,0.997-9.97,0.0998-9.98μg/mL,and the linear coefficients were 0.9996,0.9980,0.9997,and 0.9999,respectively;the average recoveries were 100.92%,100.54%,101.14%,100.93%,respectively.The relative standard deviations of determination results were less than 5.0%(n=6).This method has the advantages of simple pretreatment,short analysis time and accurate detection results,and is suitable for the quality control of lipophaga Shengfa tablets.