多波长高效液相色谱法定量分析紫金砂中5种成分

Quantitative analysis of five components in the rhizome of Angelica polymorpha by RP-HPLC under different UV wavelengths

目的:建立多波长高效液相色谱法同时测定紫金砂中水合氧化前胡素内酯(1),gosferol(2),3′R-(+)-亥茅酚(3),3′-O-乙酰基亥茅酚(4)和异欧前胡素(5)含量的分析方法。方法:紫金砂药材粉末经超声提取,HPLC-DAD检测,Agilent Eclipse XDB-C18色谱柱(4.6mm×250mm,5μm);流动相为甲醇-水梯度洗脱[55∶45(0min)～65∶35(25min)～95∶5(35min)];流速1.0mL·min-1,检测波长312nm(1),306nm(2),300nm(3),294nm(4)及310nm(5)。结果:上述5种成分线性方程分别为Y=1.81×103X+7.93×102(r=0.9996),Y=2.49×103X-2.17×102(r=0.9993),Y=2.02×103X-1.42×102(r=0.9991),Y=1.57×103X-0.66×102(r=0.9997),Y=2.65×103X-1.47×102(r=0.9996);平均回收率分别为99.7%(RSD0.57%),100.1%(RSD1.3%),100.0%(RSD1.6%),99.6%(RSD1.3%),99.2%(RSD0.59%);方法精密度,重复性,样品稳定性均符合定量分析要求。结论:该定量分析方法可用于紫金砂药材的质量控制。

A HPLC method was developed for simultaneouly quantitative analyses of aviprin （1）, gosferol （2）, 3′R-（＋）-hamaudol （3）, 3′-O-acetylhamaudol （4） and iso-imperatorin （5） in the rhizome of Angelica polymorpha. The analysis was performed at 25 ℃ on an Agilent Eclipse XDB-C18 analytical column （4.6 mm×250 mm, 5 μm） with the mobile phase of methanol and H2O in gradient elution [ 55∶45 （0 min）-65∶35 （25 min）-95∶5 （35 min） ]. And the flow rate was 1.0 mL min-1 with the detection wavelengths of 312 nm （1）, 306 nm （2）, 300 nm （3）, 294 nm （4） and 310 nm （5）. Consequently, the reqresion equations were Y=1.81×103X＋7.93×102（r=0.999 6）, Y=2.49×103 X-2.17×102 （r=0.999 3）, Y=2.02 ×103X-1.42×102 （r=0.999 1）, Y=1.57×103X-0.66×102 （r=0.999 7）, Y=2.65×103X-1.47×102 （r=0.999 6）. And the average recoveries were 99.7% （RSD 0.57%）, 100.1% （RSD 1.3%）, 100.0% （RSD 1.6%）, 99.6% （RSD 1.3%）, 99.2% （RSD 0.59%）, respectively. The precision, repeatability and stability were all consistent with the request of quantitative analysis. The contents of compound 1-5 in A. polymorpha were determined as 0.525%, 0.044%, 0.046%, 0.043%, 0.15%, respectively. Accordingly, this quantitative analysis method is good for the quality control of A. polymorpha.