摘要
目的采用高效液相色谱法同时测定荷丹片中荷叶碱、丹参酮ⅡA、补骨脂素和异补骨脂素的含量。方法采用50%乙醇超声提取,在色谱柱Agilent SB-Aq C18(4.6 mm×250 mm,5μm)上进行分离,柱温为25℃,流动相:A相为水-乙腈-三乙胺-冰醋酸(355∶30∶9∶3.9);B相:乙腈,梯度洗脱:0~11 min,30%B^20%B,11~18 min,20%B^20%B,18~30min,20%B^70%B,30~40 min,70%B^70%B,流速:1ml/min,双波长检测:245 nm(检测补骨脂素和异补骨脂素),270 nm(检测荷叶碱和丹参酮ⅡA)。结果样品中4种成分得到良好分离,荷叶碱在13.028~103.28μg/ml(r=0.9999)、丹参酮ⅡA在1.124~11.24μg/ml(r=0.9999)、补骨脂素在6.630~66.30μg/ml(r=0.9999)、异补骨脂素在6.385~63.85μg/ml(r=0.9999)范围内都呈良好线性关系;荷叶碱、丹参酮ⅡA、补骨脂素和异补骨脂素的回收率分别为95.13%、100.14%、99.76%、101.41%;RSD分别为1.07%、1.84%、1.80%、1.86%,样品溶液在12 h内稳定。结论该方法简单准确,专属性强,重复性好,可作为复方荷丹片的常规质量控制方法。
Objective To develop an high performance liquid chromatography method for simultaneous determination of nuciferine,tanshinone ⅡA,psoralen and isopsoralen in compound Hedan pills.Methods The determination was carried out over an Agilent SB-Aq C18（4.6 mm ×250 mm,5 μm） at the temperature 25℃.The mobile phase consisted of（A） H2O-ACN-TEA-HAc（355∶30∶9∶3.9）（B） ACN solution with the gradient elution 0-11 min,30%B-20%B,11-18 min,20%B-20%B,18-30 min,20%B-70%B,30-40 min,70%B-70%B.The flow rate was 1 ml/min,and the detection wavelength was set at 245 nm（detecting psoralen and isopoaln） and 322 nm（detecting nuciferine and tanshinone ⅡA）.Results The method showed a good linear relationship within the range of 13.028-103.28 μg/ml for nuciferine（r=0.9999）,1.124-11.24 μg/ml for tanshinone ⅡA（r=0.9999）,6.630-66.30 μg/ml for psoralen（r=0.9999） and 6.385-63.85 μg/ml for isopsoralen（r=0.9999）.The average recovery was 95.13%（RSD was 1.07%）for nuciferine,100.14%（RSD was 1.84%） for tanshinone ⅡA,99.76%（RSD was 1.80%） for psoralen and 101.41%（RSD was 1.86%） for isopsoralen.The sample solution was stable within 12 h.Conclusion The method is simple,accurate,sensitive,and reproducible to test major ingredients in Hedan pills.
出处
《解放军药学学报》
CAS
2011年第1期57-60,共4页
Pharmaceutical Journal of Chinese People's Liberation Army
关键词
高效液相色谱法
荷丹片
补骨脂素
异补骨脂素
荷叶碱
丹参酮ⅡA
high performance liquid chromatography
compound Hedan pills
nuciferine
tanshinone ⅡA
psoralen
isopsoralen
