丹参片的超高效液相色谱指纹图谱
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摘要
目的运用超高效液相色谱法对丹参片进行指纹图谱研究,为全面评价丹参片的整体质量提供参考。方法采用UPLC法,色谱柱为Waters ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm),以0.2%磷酸溶液(A)-乙腈(B)为流动相,梯度洗脱(0～10 min,4%B→18%B; 10～15 min,18%B→33%B; 15～19 min,33%B→49%B; 19～37 min,49%B→79%B);柱温19℃,样品管理器温度3.5℃;流速为0.25 mL/min;以丹酚酸B为参照峰,检测波长280 nm。结果建立了丹参片的UPLC指纹图谱共有模式,确定了13个峰为共有峰,所有样品的相似度均在0.900以上;指认了其中的11个共有峰,分别为:丹参素钠、原儿茶醛、迷迭香酸、紫草酸、丹酚酸B、丹酚酸A、二氢丹参酮、隐丹参酮、丹参酮Ⅰ、熊果酸和丹参酮ⅡA。结论所建立的方法能在30 min内检测丹参片中的多种成分,操作简便、快速,能全面控制丹参片的整体质量。
Objective To establish a UPLC method for fingerprints analysis of Danshen tablets,and provide reference for comprehensive evaluation of Danshen tablets.Methods UPLC method was adopted.The determination was performed on Waters ACQUITY UPLC BEH C18(2.1 mm × 50 mm,1.7 μm) column with mobile phase consisted of 0.2% Phosphoric acid(A)-acetonitrile(B) by a gradient eluted program(0 ～ 10 min,4% B→18% B;10 ～ 15 min,18% B→33% B;15 ～ 19 min,33% B→49% B;19 ～ 37 min,49% B→79%B) with a flow rate of 0.25 mL/min at 19℃.Sample manager temperature is 3.5 ℃.The detection wavelength was 280 nm with salvianolic acid B as the reference peak.Restults The standard fingerprint was established,and the overall similarity of all samples exceeded0.900.Moreover,13 common peaks were found.Among them,11 peaks were identified,including tanshinol,protocatechuic aldehyde,rosmarinci acid,lithospermic acid,salvianolic acid B,salvianolic acid A,dihydrotanshinone,cryptotanshinone,tanshinone Ⅰ,ursolic acid,tanshinone ⅡA.Conclusion This method is simple,rapid,and can be used to detect the multiple active ingredients in Danshen tablets within 30 min.So it can be used to evaluate the quality uniformity of Danshen tablets.
Objective To establish a UPLC method for fingerprints analysis of Danshen tablets,and provide reference for comprehensive evaluation of Danshen tablets.Methods UPLC method was adopted.The determination was performed on Waters ACQUITY UPLC BEH C18(2.1 mm × 50 mm,1.7 μm) column with mobile phase consisted of 0.2% Phosphoric acid(A)-acetonitrile(B) by a gradient eluted program(0 ～ 10 min,4% B→18% B;10 ～ 15 min,18% B→33% B;15 ～ 19 min,33% B→49% B;19 ～ 37 min,49% B→79%B) with a flow rate of 0.25 mL/min at 19℃.Sample manager temperature is 3.5 ℃.The detection wavelength was 280 nm with salvianolic acid B as the reference peak.Restults The standard fingerprint was established,and the overall similarity of all samples exceeded0.900.Moreover,13 common peaks were found.Among them,11 peaks were identified,including tanshinol,protocatechuic aldehyde,rosmarinci acid,lithospermic acid,salvianolic acid B,salvianolic acid A,dihydrotanshinone,cryptotanshinone,tanshinone Ⅰ,ursolic acid,tanshinone ⅡA.Conclusion This method is simple,rapid,and can be used to detect the multiple active ingredients in Danshen tablets within 30 min.So it can be used to evaluate the quality uniformity of Danshen tablets.
引文
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[10]李倩,刘伟,罗祖良,等.一测多评法测定丹参中丹参酮ⅡA、隐丹参酮、丹参酮Ⅰ、二氢丹参酮Ⅰ的含量[J].中国中药杂志,2012,37(6):824-828.
[11]郑江萍,叶政德,杨光义.丹参配方颗粒HPLC指纹图谱研究[J].海峡药学,2016,28(9):45-49.
[12]时荣同,张清文,姚惠,等. HPLC法测定注射用丹参多酚酸盐中丹参乙酸镁的含量[J].安徽医药,2016,20(3):466-468.
[13]高杨,王彬,秦昆明,等.正交法优选丹参提取工艺研究[J].安徽医药,2015,19(12):2276-2279.
[14]张雪,褚文静,黄喜茹,等.反相高效液相色谱二极管阵列检测法同时测定丹参饮片中5种水溶性成分[J].理化检验-化学分册,2010,46(11):1323-1325.
[15]孙棣,刘文英,梁彩. HPLC法同时测定丹参片中4种有效成分的含量[J].中国医科大学学报,2007,38(1):51-54.
[16]周维,胡昌江,戴德荣,等.丹参饮片、标准水煎剂、配方颗粒HPLC特征图谱相关性研究[J].中国现代中药,2016,18(9):1100-1102,1113.
[2]许虎,刘训红,傅兴圣,等.高效毛细管电泳法同时测定丹参饮片中5种酚酸类成分[J].中国药学杂志,2012,47(20):1661-1664.
[3]张青云,崔田.丹参片脂溶性成分HPLC指纹图谱研究[J].淮海医药,2011,29(1):66-67.
[4]李耿,孟繁蕴,杨洪军,等. UPLC法同时测定丹参中11种成分的含量[J].中国药房,2014,25(19):1766-1768.
[5]张琚,程月发,张爱兵,等.不同厂家的丹参片和丹参胶囊中四种活性成分的高效液相色谱法比较分析[J].时珍国医国药,2012,23(11):2790-2791.
[6]何昱,成金乐,徐吉银,等. HPLC-DAD同时测定丹参中原儿茶醛、丹酚酸B、隐丹参酮、丹参酮ⅡA四种成分的含量[J].世界科学技术—中医药现代化,2011,13(4):688-692.
[7]周晓希,孔羽,魏宇昆,等. RP-HPLC-DAD同时测定丹参及丹参片中6种水溶性成分的含量[J].中药材,2014,37(2):337-339.
[8]迟栋,贾荷丽. HPLC研究裕丹参水煎液指纹图谱[J].光明中医,2013,28(3):481-482.
[9]宋建平,许虎,刘训红,等.丹参HPCE—DAD指纹图谱的研究[J].中药材,2012,35(9):1414-1417.
[10]李倩,刘伟,罗祖良,等.一测多评法测定丹参中丹参酮ⅡA、隐丹参酮、丹参酮Ⅰ、二氢丹参酮Ⅰ的含量[J].中国中药杂志,2012,37(6):824-828.
[11]郑江萍,叶政德,杨光义.丹参配方颗粒HPLC指纹图谱研究[J].海峡药学,2016,28(9):45-49.
[12]时荣同,张清文,姚惠,等. HPLC法测定注射用丹参多酚酸盐中丹参乙酸镁的含量[J].安徽医药,2016,20(3):466-468.
[13]高杨,王彬,秦昆明,等.正交法优选丹参提取工艺研究[J].安徽医药,2015,19(12):2276-2279.
[14]张雪,褚文静,黄喜茹,等.反相高效液相色谱二极管阵列检测法同时测定丹参饮片中5种水溶性成分[J].理化检验-化学分册,2010,46(11):1323-1325.
[15]孙棣,刘文英,梁彩. HPLC法同时测定丹参片中4种有效成分的含量[J].中国医科大学学报,2007,38(1):51-54.
[16]周维,胡昌江,戴德荣,等.丹参饮片、标准水煎剂、配方颗粒HPLC特征图谱相关性研究[J].中国现代中药,2016,18(9):1100-1102,1113.
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