【摘要】 目的建立白术、白芍、白术-白芍、痛泻要方中白术内酯Ⅰ、Ⅱ、Ⅲ,芍药苷、芍药内酯苷的HPLC-PDA色谱分析方法,同时测定5种成分在单味药、药对、复方中的含量,为探究配伍对化学成分的影响提供科学依据。方法采用Thermo Fisher C18（4.6 mm×150 mm,5μm）色谱柱,以乙腈（A）-水（B）为流动相梯度洗脱;运行时间:32 min;柱温:30℃;流速:1 ml·min-1;检测波长:白术内酯Ⅰ及白术内酯Ⅲ为222 nm,白术内酯Ⅱ为278 nm,芍药苷、芍药内酯苷为232 nm;进样量:10μl。结果对检测结果进行线性考察,以峰面积（Y）与浓度（X）进行线性回归,白术内酯Ⅰ、Ⅱ、Ⅲ,芍药苷、芍药内酯苷的线性范围分别为0.008 0⁰.320 0μg（r₁=0.999 9）、0.004 1⁰.160 0μg（r₂=0.999 8）、0.210 0⁰.840 0μg（r₃=0.999 7）、1.750 0⁷0.000 0μg（r₄=0.999 8）、1.000 0⁴0.000 0μg（r5=0.999 6）;加样回收试验、精密度试验、重复性试验良好,稳定性试验证明在24 h内稳定,结果准确可靠。在单味药、药对与复方中,5种有效成分含量的高低顺序依次是芍药苷>芍药内酯苷>白术内酯Ⅲ>白术内酯Ⅰ>白术内酯Ⅱ。比较白术与白芍配伍前后的含量发现,白术内酯Ⅰ、Ⅱ、Ⅲ的含量较配伍前均有所升高,而芍药苷和芍药内酯苷的含量较配伍之前的含量均降低;比较药对与复方中5种成分的含量发现,白术内酯Ⅰ的含量药对较复方明显升高,白术内酯Ⅱ、Ⅲ,芍药苷、芍药内酯苷的含量明显降低。结论该法可同时对单味药、药对以及复方的质量控制进行评价;通过比较单味药、药对、复方中有效成分含量的变化,表明配伍可以对药物的有效成分产生影响。更多还原

【Abstract】 Objective To establish a high performance liquid chromatography-photodiode array（ HPLC-PDA） method for the simultaneous determination of five effective components（ atractylenolide Ⅰ,atractylenolide Ⅱ,atractylenolide Ⅲ,albiflorin and paeoniflorin）,detect their contents in Baizhu（ Atractylodis Macrocephalae Rhizoma）,Baishao（ Paeoniae Radix Alba）,couplet medicines and compound recipe（ Tongxie Yao Recipe）,and provide scientific basis for research on effects of compatibility on chemical components. Methods The separation was performed on a Thermo Fisher C18 column（ 4.6 mm×150 mm,5 μm）by gradient elution of acetonitrile（ A）-water（ B） as the mobile phase at flow rate of 1 ml·min-1,with running time of 32 minutes and column temperature at 30℃. The detection wavelength was set at 222 nm for atractylenolideⅠand Ⅲ,278 nm for atractylenolide Ⅱ and 232 nm for albiflorin and paeoniflorin. The volume of sample injection was 10 μl. Results Linear investigation on detection results was performed by linear regression with peak area（ Y） and concentration（ X）. The linear ranges of atractylenolideⅠ,Ⅱ,Ⅲ,paeoniflorin and albiflorin were at 0.008 0-0.320 0 μg（ r₁= 0.999 9）,0.004 1-0.160 0 μg（ r₂= 0.999 8）,0.210 0-0.840 0 μg（ r₃= 0.999 7）,1.750 0-70.000 0 μg（ r₄= 0.999 8）,1.000 0-40.000 0 μg（ r5= 0.999 6）,respectively. The sample recovery test,precision test and repeatability test performed well. The stability test verified the good stability within 24 hours,which meant that the results were accurate and reliable. The contents of the five effective ingredients in single drug,couplet medicines and compound recipe were paeoniflorin > albiflorin > atractylenolide Ⅲ > atractylenolide Ⅰ >atractylenolide Ⅱ. Compared with the single drug,the contents of atractylenolideⅠ,Ⅱ and Ⅲ were increased after the compatibility of Baizhu and Baishao,but the contents of paeoniflorin and albiflorin were decreased. For the comparison between the couplet medicines and compound recipe,the content of atractylenolideⅠin the couplet medicines was obviously higher than that in the compound recipe,and the contents of atractylenolide Ⅱ,atractylenolide Ⅲ,paeoniflorin and albiflorin in the couplet medicines were obviously lower than those in the compound recipe. Conclusion This method can be used for the quality control of single drug,couplet medicines and compound recipe. Through the comparison of contents of effective ingredients in single drug,couplet medicines and compound recipe,it suggests the impacts of compatibility on effective ingredients of drugs.更多还原