HPLC-PDA同时测定白术-白芍单味药、药对、复方中5种有效成分的含量  

Simultaneous determination of five effective ingredients of Baizhu( Atractylodis Macrocephalae Rhizoma) and Baishao( Paeoniae Radix Alba) in single drug,couplet medicines and compound recipe by HPLC-PDA

作　　者：王艳宏[1] 张秋樾 历凯 赵娟萍[1] 王智[3] 赵雪[1] 齐笑 旺建伟[4] WANG Yanhong;ZHANG Qiuyue;LI Kai;ZHAO Juanping;WANG Zhi;ZHAO Xue;QI Xiao;WANG Jianwei(College of Pharmacy, Heilongjiang University of Chinese Medicine, Harbin 150040, China;Harbin Food and Drug Administration, Harbin 150036, China;Second Affiliated Hospital of Heilongjiang University of Chinese Medicine, Harbin 150001, China;School of Basic Medical Science, Heilongjiang University of Chinese Medicine, Harbin 150040, China)

机构地区：[1]黑龙江中医药大学药学院,黑龙江哈尔滨150040 [2]黑龙江省哈尔滨市食品药品监督管理局,黑龙江哈尔滨150036 [3]黑龙江中医药大学附属第二医院,黑龙江哈尔滨150001 [4]黑龙江中医药大学基础医学院,黑龙江哈尔滨150040

出　　处：《上海中医药杂志》2018年第4期101-106,共6页Shanghai Journal of Traditional Chinese Medicine

基　　金：国家自然科学基金面上项目(81573870);中国博士后科学基金第八批特别资助项目(2015T80376);黑龙江省自然科学基金面上项目(H2015020);黑龙江中医药大学优秀创新人才支持计划(优秀青年学术带头人)资助项目(051217)

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 0~0.320 0μg(r_1=0.999 9)、0.004 1~0.160 0μg(r_2=0.999 8)、0.210 0~0.840 0μg(r_3=0.999 7)、1.750 0~70.000 0μg(r_4=0.999 8)、1.000 0~40.000 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。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 m

关 键 词：痛泻要方 白术 白芍 HPLC-PAD 有效成分 

分 类 号：R284.1[医药卫生—中药学]