延胡索炮制前后多组分质量控制方法的研究
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摘要
[目的]建立超高效液相色谱法(UPLC)同时测定延胡索药材中四氢非洲防己碱、原阿片碱、四氢黄连碱、非洲防己碱、延胡索乙素、盐酸小檗碱、盐酸巴马汀、去氢紫堇碱8种生物碱含量的方法,并对延胡索生品及炮制品进行测定。[方法]采用UPLC检测方法,ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm),乙腈(B)-0.2%甲酸水溶液,梯度洗脱,流速:0.3 mL/min,柱温55℃,检测波长280 nm。[结果]四氢非洲防己碱,原阿片碱、四氢黄连碱、非洲防己碱、延胡索乙素、盐酸小檗碱、盐酸巴马汀、去氢紫堇碱在0.395～98.8、0.4～100.2、0.99～247.5、0.197～49.4、1.004～251、0.198～49.5、0.398～99.6、1～250μg/mL浓度范围内线性良好,平均加样回收率在98.10%～100.87%,RSD≤1.94(n=6)。[结论] UPLC所建立的方法简便、快速、准确,可应用于延胡索药材中多种成分含量测定,为延胡索药材质量控制提供更加科学、便捷的方法。
[Objective] To establish an UPLC method for the simultaneous determination of eightalkaloids(tetrahydrocolumbamine,protopine,tetrahydrocoptisine,columbamine,tetrahy-dropalmatine,berberine hydrochloride,palmatine hydrochloride and dehydrocorydaline)in corydalis yanhusuofrom the products and processed products. [Methods] The separationwas performed on an ACQUITY UPLCBEH C18(100 mm × 2.1 mm,1.7 μm) columnin the UPLC method. The mobile phases consisted of acetonitrile(B) and 0.2% formic acid aqueous solutionwith gradient elution. The flow rate was 0.3 mL/min,the column temperature was 55 ℃,and the detection wavelength was 280 nm. [Results] Good linearities oftetrahydrocolumbamine,protopine,tetrahydrocoptisine,columbamine,tetrahydropalmatine,berberine hydrochloride,palmatine hydrochloride and dehydrocorydaline were achievedwithin the range of 0.395～98.8、0.4～100.2、0.99～247.5、0.197～49.4、1.004～251、0.198～49.5、0.398～99.6、1 ～250 μg/mL,respectively. The average recoveries were in the range of 98.10%-100.87%,RSD ≤1.94(n =6).[Conclusion] The method established by UPLC is simple,rapid and accurate,and it can be applied to the determination of various components in Corydalis yanhusuo,and provide a more scientific and convenient method for the quality control of Corydalis yanhusuo.
[Objective] To establish an UPLC method for the simultaneous determination of eightalkaloids(tetrahydrocolumbamine,protopine,tetrahydrocoptisine,columbamine,tetrahy-dropalmatine,berberine hydrochloride,palmatine hydrochloride and dehydrocorydaline)in corydalis yanhusuofrom the products and processed products. [Methods] The separationwas performed on an ACQUITY UPLCBEH C18(100 mm × 2.1 mm,1.7 μm) columnin the UPLC method. The mobile phases consisted of acetonitrile(B) and 0.2% formic acid aqueous solutionwith gradient elution. The flow rate was 0.3 mL/min,the column temperature was 55 ℃,and the detection wavelength was 280 nm. [Results] Good linearities oftetrahydrocolumbamine,protopine,tetrahydrocoptisine,columbamine,tetrahydropalmatine,berberine hydrochloride,palmatine hydrochloride and dehydrocorydaline were achievedwithin the range of 0.395～98.8、0.4～100.2、0.99～247.5、0.197～49.4、1.004～251、0.198～49.5、0.398～99.6、1 ～250 μg/mL,respectively. The average recoveries were in the range of 98.10%-100.87%,RSD ≤1.94(n =6).[Conclusion] The method established by UPLC is simple,rapid and accurate,and it can be applied to the determination of various components in Corydalis yanhusuo,and provide a more scientific and convenient method for the quality control of Corydalis yanhusuo.
引文
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[16]沈小月,宋敏,杭太俊.LC-MS法鉴定桑叶中生物碱类成分[J].药物分析杂志,2016,36(10):1737-1744.
[17]李翠翠.超高效液相色谱法在西药分析中的应用探讨[J].科学与财富,2014,(4):361~362.
[18]陈静,郑荣,季申,等.超高效液相色谱法同时测定化妆品中的19种喹诺酮类抗生素[J].分析化学研究简报,2013,41(6):931-935.
[19]张娜,王国祥,Abacar Jose Daniel,等.超高效液相色谱法分析稻米酚酸化合物组分及其含量[J]中国农业科学,2015,48(9):1718-1726.
[20]林武霖,王如伟,孙柳燕.延胡索质量控制的研究进展[J].中草药,2011,42(2):409-412.
[21]吴雪松,许浚,张喜民,等.元胡止痛方的化学成分及药理作用研究进展[J].中草药,2015,46(7):1081-1095.
[22]窦志英,孙巍,田丽莉,等.HPLC法比较延胡索生品与不同炮制品中3种有效成分的含量[J].中药材,2007,30(4):399-401.
[23]费艳美,张玉萍,方步武.酸性染料比色法测定延胡索总生物碱的含量[J].现代中药研究与实践,2012,26(3):66.
[2]贺凯,高建莉,赵光树.延胡索化学成分、药理作用及质量控制研究进展[J].中草药,2007,38(12):1909-1912.
[3]马月光,岳显可,曹岗,等.不同产地延胡索饮片炮制前后有效成分含量的测定[J].中药材,2013,36(11):1754-1758.
[4]肖辉.不同炮制方法对延胡索中延胡索乙素含量的影响[J].中国药业,2016,25(4):29-31.
[5]罗琛艳,李浩,肖洋,等.延胡索药材及饮片UPLC质量控制方法[J].天津中医药大学学报[J].2015,34(6):357-360.
[6]高建莉,陈兆飞,石俊敏,等.延胡索中5种生物碱的含量测定及稳定性研究[J].中国药房,2012,23(15):1386-1388.
[7]雷云,李先端,杨洪军,等.基于成分分析和活性评价的延胡索醋制的研究[J].中草药,2013,44(21):2992-2996.
[8]毕福钧,林彤.RP-HPLC法同时测定醋延胡索配方颗粒中7种生物碱[J].中草药2016,47(4):606-609.
[9]赵新娟,沈梅,石俊敏,等.高效液相色谱法测定延胡索药材中7种异喹啉类生物碱的含量[J].天然产物研究与开发,2015,27(12):2074-2078.
[10]陈东东,毛坤军,李祥,等.HPLC法比较延胡索炮制前后7个生物碱成分的含量[J].药物分析杂志,2015,35(9):1591-1595.
[11]印成霞.超高效液相色谱法在药物分析中的应用研究[J].中国实用医药,2013,8(23):230~231.
[12]金高娃,章飞芳,薛兴亚.超高速液相色谱在复杂体系中药分离分析中的应用[J].世界科学技术中医药现代化,2006,8(3):106-111.
[13]Wren SAC,Tchelitcheff P.Use of ultra-performance liquidchromatography in pharmaceu tical developm ent[J].JChrom atogr A,2006(1119):140-146.
[14]Novakova LM atysova L,Solich P.Advantages of application of UPLC in pharmaceutica lanalysis[J].Talanta,2006,68:908-918.
[15]肖竦.毛细管电泳测定钩藤中钩藤碱、异钩藤碱、去氢钩藤碱的含量[J].现代化工,2011,31(8):90-92.
[16]沈小月,宋敏,杭太俊.LC-MS法鉴定桑叶中生物碱类成分[J].药物分析杂志,2016,36(10):1737-1744.
[17]李翠翠.超高效液相色谱法在西药分析中的应用探讨[J].科学与财富,2014,(4):361~362.
[18]陈静,郑荣,季申,等.超高效液相色谱法同时测定化妆品中的19种喹诺酮类抗生素[J].分析化学研究简报,2013,41(6):931-935.
[19]张娜,王国祥,Abacar Jose Daniel,等.超高效液相色谱法分析稻米酚酸化合物组分及其含量[J]中国农业科学,2015,48(9):1718-1726.
[20]林武霖,王如伟,孙柳燕.延胡索质量控制的研究进展[J].中草药,2011,42(2):409-412.
[21]吴雪松,许浚,张喜民,等.元胡止痛方的化学成分及药理作用研究进展[J].中草药,2015,46(7):1081-1095.
[22]窦志英,孙巍,田丽莉,等.HPLC法比较延胡索生品与不同炮制品中3种有效成分的含量[J].中药材,2007,30(4):399-401.
[23]费艳美,张玉萍,方步武.酸性染料比色法测定延胡索总生物碱的含量[J].现代中药研究与实践,2012,26(3):66.