HPLC法测定强筋健骨丸中3种乌头原碱的含量
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摘要
目的建立强筋健骨丸的含量测定方法。方法以君药制川乌、制草乌中苯甲酰乌头原碱、苯甲酰次乌头原碱及苯甲酰新乌头原碱为目标成分,采用HPLC法,色谱柱Ultimate XB-C_(18)(250mm×4.6mm,5μm);流动相:乙腈(A)-0.1mol·L~(-1)醋酸铵溶液(B);流速:1.0mL·min~(-1);检测波长:235nm。结果苯甲酰新乌头原碱、苯甲酰乌头原碱和苯甲酰次乌头原碱质量浓度分别在7.580～121.280(r_1=0.999 9),1.576～25.216(r_2=0.999 8)和7.732～123.712(r_3=0.999 9)mg·L~(-1)范围内线性关系均良好,回收率分别为100.1%,100.0%和99.8%,RSD值分别为0.8%,1.5%和0.6%。结论该方法结果准确、稳定、可靠,能用于强筋健骨丸中苯甲酰新乌头原碱、苯甲酰乌头原碱及苯甲酰次乌头原碱的含量测定,可有效控制产品质量。
Objective To establish a method for the determination of Qiangjin Jiangu Pills.Methods The target components were benzoylaconine,benzoylhypaconine and benzoylmesaconine in the monarch medicine Radix Aconiti preparata and Radix Aconiti Kusnezoffii preparata.HPLC was used with Ultimate XB-C_(18)(250mm×4.6mm,5μm)as the column,and acetonitrile(A)-0.1mol·L~(-1)ammonium acetate solution(B)as the mobile phase.The flow rate was 1.0mL·min~(-1 )and the detection wavelength was 235nm.Results The linear relationships of benzoylmesaconine in the mass concentration range of 7.580-121.280mg·L~(-1)(r_1=0.999 9),benzoylaconine in the range of 1.576-25.216mg·L~(-1)(r_2=0.999 8)and benzoylhypaconine in the range of 7.732-123.712mg·L~(-1)(r_3=0.999 9)were good.The recovery rates were 100.1%,100.0% and 99.8%,with RSD of 0.8%,1.5% and 0.6%,respectively.Conclusion The method is accurate,stable and reliable,and can be used to determine the content of benzoylaconine,benzoylhypaconine and benzoylmesaconine in Qiangjin Jiangu Pills and control the product quality effectively.
Objective To establish a method for the determination of Qiangjin Jiangu Pills.Methods The target components were benzoylaconine,benzoylhypaconine and benzoylmesaconine in the monarch medicine Radix Aconiti preparata and Radix Aconiti Kusnezoffii preparata.HPLC was used with Ultimate XB-C_(18)(250mm×4.6mm,5μm)as the column,and acetonitrile(A)-0.1mol·L~(-1)ammonium acetate solution(B)as the mobile phase.The flow rate was 1.0mL·min~(-1 )and the detection wavelength was 235nm.Results The linear relationships of benzoylmesaconine in the mass concentration range of 7.580-121.280mg·L~(-1)(r_1=0.999 9),benzoylaconine in the range of 1.576-25.216mg·L~(-1)(r_2=0.999 8)and benzoylhypaconine in the range of 7.732-123.712mg·L~(-1)(r_3=0.999 9)were good.The recovery rates were 100.1%,100.0% and 99.8%,with RSD of 0.8%,1.5% and 0.6%,respectively.Conclusion The method is accurate,stable and reliable,and can be used to determine the content of benzoylaconine,benzoylhypaconine and benzoylmesaconine in Qiangjin Jiangu Pills and control the product quality effectively.
引文
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[4]马云娜,徐远涛,焦洁,等.反相高效液相色谱法同时测定骨刺消痛胶囊中3种单酯型生物碱的含量[J].中南药学,2018,16(3):412-415.
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[7]李谦,过立农,郑健,等.乌头属药用植物的研究进展[J].药物分析杂志,2016,36(7):1129-1149.
[8]熊亮,彭成,缪璐琳,等.基于“毒-效整合分析思路”探讨有毒中药附子的物质基础[J].世界中医药,2017,12(11):2568-2578,2584.
[9]杨苗苗,杨霖,李孝栋.乌头安全有效性研究进展及其临床应用前景[J].药学研究,2018,37(3):125-133,155.
[10]黄志芳,易进海,陈东安,等.制川乌HPLC特征图谱研究和6种酯型生物碱的含量测定[J].药物分析杂志,2011,31(2):217-221.
[11]徐硕,梁晓丽,李琼,等.中药附子的研究进展[J].西北药学杂志,2017,32(2):248-封4.
[12]张晓东,杜晓鹂.高效液相串联质谱法测定制草乌中单酯型生物碱的含量[J].内蒙古医科大学学报,2017,39(2):152-154,158.
[13]倪洁.HPLC法测定中药饮片制川乌、制草乌中乌头碱、次乌头碱的含量[J].亚太传统医药,2013,9(8):29-30.
[14]李耿,张敏敏,赵亚,等.HPLC法同时测定乌头属不同药材4种生物碱的含量[J].中药材,2012,35(6):927-930.
[15]郑杭生,冯年平.中药饮片制川乌、制草乌中乌头碱、次乌头碱的HPLC测定[J].药物分析杂志,2005,25(1):34-36.
[2]国家药典委员会.中国药典:2015年版:一部[S].2015:39,237.
[3]黄茜,孙明丽,李腾飞,等.乌头生物碱镇痛作用及机制研究进展[J].神经药理学报,2017,7(3):21-32.
[4]马云娜,徐远涛,焦洁,等.反相高效液相色谱法同时测定骨刺消痛胶囊中3种单酯型生物碱的含量[J].中南药学,2018,16(3):412-415.
[5]邓广海.川乌、草乌炮制工艺及指纹图谱的研究[D].广州:广州中医药大学,2011.
[6]陈巧玲.川乌、草乌、附子及其复方制剂中乌头类生物碱的含量测定研究概况[J].华西药学杂志,1999,14(2):114-116.
[7]李谦,过立农,郑健,等.乌头属药用植物的研究进展[J].药物分析杂志,2016,36(7):1129-1149.
[8]熊亮,彭成,缪璐琳,等.基于“毒-效整合分析思路”探讨有毒中药附子的物质基础[J].世界中医药,2017,12(11):2568-2578,2584.
[9]杨苗苗,杨霖,李孝栋.乌头安全有效性研究进展及其临床应用前景[J].药学研究,2018,37(3):125-133,155.
[10]黄志芳,易进海,陈东安,等.制川乌HPLC特征图谱研究和6种酯型生物碱的含量测定[J].药物分析杂志,2011,31(2):217-221.
[11]徐硕,梁晓丽,李琼,等.中药附子的研究进展[J].西北药学杂志,2017,32(2):248-封4.
[12]张晓东,杜晓鹂.高效液相串联质谱法测定制草乌中单酯型生物碱的含量[J].内蒙古医科大学学报,2017,39(2):152-154,158.
[13]倪洁.HPLC法测定中药饮片制川乌、制草乌中乌头碱、次乌头碱的含量[J].亚太传统医药,2013,9(8):29-30.
[14]李耿,张敏敏,赵亚,等.HPLC法同时测定乌头属不同药材4种生物碱的含量[J].中药材,2012,35(6):927-930.
[15]郑杭生,冯年平.中药饮片制川乌、制草乌中乌头碱、次乌头碱的HPLC测定[J].药物分析杂志,2005,25(1):34-36.