葛根芩连丸UPLC指纹图谱建立及7种成分测定
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摘要
目的建立葛根芩连丸(葛根、黄芩、黄连、炙甘草)UPLC指纹图谱,并测定葛根素、黄芩素、巴马汀、汉黄芩素、大豆苷、大豆苷元、药根碱的含有量。方法该药物70%甲醇提取液的分析采用Waters ACQUITY UPLC~ BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm);甲醇-0.1%冰醋酸为流动相,梯度洗脱;体积流量0.3 m L/min;检测波长260 nm;柱温30℃。结果 10批样品指纹图谱中有25个共有峰,相似度大于0.98。7种成分在各自范围内线性关系良好(r>0.999 0),平均加样回收率98.99%~103.6%,RSD 1.13%~2.03%。结论该方法简便可靠,重复性好,可用于葛根芩连丸的质量控制。
AIM To establish the UPLC fingerprints of Gegen Qinlian Pills( Puerariae lobatae Radix,Scutellariae Radix,Coptidis Rhizoma and Glycyrrhizae Radix et Rhizoma Praeparata cum Melle) and to determine the contents of puerarin,baicalein,palmatine,wogonin,daidzin,daidzein and jateorhizine. METHODS The analysis of 70% methanol extract of this drug was performed on a 30 ℃ thermostatic Waters ACQUITY UPLC~ BEH C_(18) column,with the mobile phase comprising of methanol-0. 1% glacial acetic acid flowing at 0. 3 m L/min in a gradient manner,and the detection wavelength was set at 260 nm. RESULTS There were twenty-five common peaks in the fingerprints of ten batches of samples with the similarities of more than 0. 98. Seven constituents showed good linear relationships within their own ranges( r > 0. 999 0),whose average recoveries were 98. 99%-103. 6% with the RSDs of 1. 13%-2. 03%. CONCLUSION This simple,reliable and reproducible method can be used for the quality control of Gegen Qinlian Pills.
AIM To establish the UPLC fingerprints of Gegen Qinlian Pills( Puerariae lobatae Radix,Scutellariae Radix,Coptidis Rhizoma and Glycyrrhizae Radix et Rhizoma Praeparata cum Melle) and to determine the contents of puerarin,baicalein,palmatine,wogonin,daidzin,daidzein and jateorhizine. METHODS The analysis of 70% methanol extract of this drug was performed on a 30 ℃ thermostatic Waters ACQUITY UPLC~ BEH C_(18) column,with the mobile phase comprising of methanol-0. 1% glacial acetic acid flowing at 0. 3 m L/min in a gradient manner,and the detection wavelength was set at 260 nm. RESULTS There were twenty-five common peaks in the fingerprints of ten batches of samples with the similarities of more than 0. 98. Seven constituents showed good linear relationships within their own ranges( r > 0. 999 0),whose average recoveries were 98. 99%-103. 6% with the RSDs of 1. 13%-2. 03%. CONCLUSION This simple,reliable and reproducible method can be used for the quality control of Gegen Qinlian Pills.
引文
[1]罗奇志,戴开金,马安德,等.葛根芩连汤及微丸中葛根素、大豆苷元的HPCE分析[J].药物分析杂志,2004,24(1):11-13.
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[11]石俊敏,管佳,张庆文,等.超高效液相色谱在药物分析中的应用[J].药物分析杂志,2008,28(9):1583-1588.
[12]曹进,饶毅,沈群,等.中药注射剂指纹图谱分析[J].世界科学技术(中医药现代化),2001,3(4):20-24,82.
[13]屠鹏飞,高效液相色谱法制定中药材和中药注射剂特征指纹图谱的探讨[J].中成药,2000,22(7):516.
[14]陈佳,王钢力,姚令文,等.超高效液相色谱(UPLC)在药物分析领域中的应用[J].药物分析杂志,2008,28(11):1976-1981.
[15]吴莎,王雪,吴亚男,等.UPLC用于热毒宁注射液中11种成分测定及其指纹图谱研究[J].中国中药杂志,2014,39(24):4804-4810.
[2]宋亚芳,苏春梅,杨红,等.HPLC同时测定葛根芩连微丸中葛根素、甘草苷、黄芩苷、盐酸小檗碱的含量[J].中国实验方剂学杂志,2013,19(2):64-67.
[3]董宏然,程琪庆,段丽颖,等.丹七软胶囊UPLC指纹图谱研究及组分鉴别[J].中成药,2016,38(1):117-122.
[4]贺祝英,吕海涛,曹佩雪,等.葛根芩连汤不同制法对葛根素含量的影响[J].中国医院药学杂志,2002,22(9):518-519.
[5]文谨,刘起华,章军,等.葛根芩连汤煮散煎煮工艺优化[J].中成药,2016,38(9):2070-2073.
[6]吴永芹,冯凯,周慧,等.HPLC法同时测定葛根芩连片中葛根素和黄芩苷的含量[J].中国药事,2012,26(3):282-284.
[7]An R,Wang Y,You L S,et al.UPLC-MS analysis for simultaneous determination of eight components in the‘Ge-GenQin-Lian’tablets[J].Chromatographia,2009,69(9-10):969-975.
[8]崔向微,张贵君,李慧,等.葛根芩连汤两种配伍比例的化学药效组分比较分析[J].中成药,2009,31(2):263-266.
[9]李强,杜思邈,张忠亮,等.中药指纹图谱技术进展及未来发展方向展望[J].中草药,2013,44(22):3095-3104.
[10]冯伟红,李春,吉丽娜,等.基于高分离度和高色谱峰纯度的红参UPLC指纹图谱研究[J].中国中药杂志,2016,41(20):3798-3804.
[11]石俊敏,管佳,张庆文,等.超高效液相色谱在药物分析中的应用[J].药物分析杂志,2008,28(9):1583-1588.
[12]曹进,饶毅,沈群,等.中药注射剂指纹图谱分析[J].世界科学技术(中医药现代化),2001,3(4):20-24,82.
[13]屠鹏飞,高效液相色谱法制定中药材和中药注射剂特征指纹图谱的探讨[J].中成药,2000,22(7):516.
[14]陈佳,王钢力,姚令文,等.超高效液相色谱(UPLC)在药物分析领域中的应用[J].药物分析杂志,2008,28(11):1976-1981.
[15]吴莎,王雪,吴亚男,等.UPLC用于热毒宁注射液中11种成分测定及其指纹图谱研究[J].中国中药杂志,2014,39(24):4804-4810.