HPLC同时测定杞菊地黄口服液12种成分
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摘要
目的建立一种快速、准确和实用的HPLC方法,用于同时测定杞菊地黄口服液中5-羟甲基糠醛(5-HMF)、莫诺苷、绿原酸、隐绿原酸、马钱苷、芍药苷、毛蕊花糖苷、木犀草苷、异绿原酸B、异绿原酸A、异绿原酸C、丹皮酚的含量。方法采用YMC ODS柱(250 mm×4.6 mm,5μm),柱温35℃,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,体积流量为1.0 mL/min,检测波长为254、325 nm,进样量10μL。结果 5-HMF、莫诺苷、绿原酸、隐绿原酸、马钱苷、芍药苷、毛蕊花糖苷、木犀草苷、异绿原酸B、异绿原酸A、异绿原酸C、丹皮酚进样量在0.08～1.60、0.12～2.40、0.09～1.80、0.06～1.20、0.10～2.00、0.30～6.00、0.01～0.20、0.01～0.20、0.01～0.20、0.005～0.10、0.005～0.10、0.01～0.20μg与峰面积呈良好的线性关系,精密度、重复性、稳定性均良好,RSD均小于3.5%,加样回收率均在96%～103%,RSD分别为2.13%、3.45%、2.86%、2.59%、3.15%、3.49%、2.19%、3.25%、2.37%、2.53%、2.91%、3.35%,测定5批样品中各成分含量稳定,所测12种成分质量浓度分别为98.56～102.56、204.28～212.10、18.53～18.89、1.95～2.05、12.31～12.54、87.01～87.12、5.35～5.43、16.08～16.15、8.69～8.72、8.89～8.95、5.12～5.19、1.87～1.94μg/m L。结论本方法可以同时测定杞菊地黄口服液中5-HMF、莫诺苷、绿原酸、隐绿原酸、马钱苷、芍药苷、毛蕊花糖苷、木犀草苷、异绿原酸B、异绿原酸A、异绿原酸C、丹皮酚的含量,适用于杞菊地黄口服液的质量控制。
Objective To establish a rapid, accurate, and practical HPLC method for simultaneous determination the content in Qiju Dihuang Oral Liquid(QDOL) of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside,luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and paeonol. Methods YMC ODS column(250 mm × 4.6 mm, 5 μm) was used, column temperature was set at 35 ℃, gradient elution with 0.1% formic acid aqueous solutionacetonitrile was used as mobile phase, flow rate was 1.0 mL/min, detection wavelength was 254 and 325 nm. The injection volume was10 μL. Results The injection amount of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin,verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, paeonol injection quality at 0.08—1.60,0.12—2.40, 0.09—1.80, 0.06—1.20, 0.10—2.00, 0.30—6.00, 0.01—0.20, 0.01—0.20, 0.01—0.20, 0.005—0.10, 0.005—0.10, and0.01—0.20 μg showed a good linear relationship with peak area, with good precision, repeatability and stability. The recovery rates of the samples were between 96% and 103%, the RSD was 2.13%, 3.45%, 2.86%, 2.59%, 3.15%, 3.49%, 2.19%, 3.25%, 2.37%, 2.53%,2.91%, and 3.35%, respectively. The content of each component of the five batches of samples was stable, and the mass concentrations range of the 12 components tested were 98.56—102.56, 204.28—212.10, 18.53—18.89, 1.95—2.05, 12.31—12.54, 87.01—87.12,5.35—5.43, 16.08—16.15, 8.69—8.72, 8.89—8.95, 5.12—5.19, and 1.87—1.94 μg/mL. Conclusion The method simltaneosly determines the content of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside,luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and paeonol in QDOL, which is suitable for the quality control of QDOL.
Objective To establish a rapid, accurate, and practical HPLC method for simultaneous determination the content in Qiju Dihuang Oral Liquid(QDOL) of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside,luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and paeonol. Methods YMC ODS column(250 mm × 4.6 mm, 5 μm) was used, column temperature was set at 35 ℃, gradient elution with 0.1% formic acid aqueous solutionacetonitrile was used as mobile phase, flow rate was 1.0 mL/min, detection wavelength was 254 and 325 nm. The injection volume was10 μL. Results The injection amount of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin,verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, paeonol injection quality at 0.08—1.60,0.12—2.40, 0.09—1.80, 0.06—1.20, 0.10—2.00, 0.30—6.00, 0.01—0.20, 0.01—0.20, 0.01—0.20, 0.005—0.10, 0.005—0.10, and0.01—0.20 μg showed a good linear relationship with peak area, with good precision, repeatability and stability. The recovery rates of the samples were between 96% and 103%, the RSD was 2.13%, 3.45%, 2.86%, 2.59%, 3.15%, 3.49%, 2.19%, 3.25%, 2.37%, 2.53%,2.91%, and 3.35%, respectively. The content of each component of the five batches of samples was stable, and the mass concentrations range of the 12 components tested were 98.56—102.56, 204.28—212.10, 18.53—18.89, 1.95—2.05, 12.31—12.54, 87.01—87.12,5.35—5.43, 16.08—16.15, 8.69—8.72, 8.89—8.95, 5.12—5.19, and 1.87—1.94 μg/mL. Conclusion The method simltaneosly determines the content of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside,luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and paeonol in QDOL, which is suitable for the quality control of QDOL.
引文
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[2]陶娜,李亚兰,项奕.杞菊地黄丸对白内障术后干眼症患者疗效,BμT,SIT及FL的影响[J].中国实验方剂学杂志,2017,23(23):166-170.
[3]黎绮雯.杞菊地黄丸联合重组成纤维细胞生长因子凝胶治疗白内障术后干眼症的临床研究[J].中医药导报,2016,22(6):93-95.
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[5]李桂本,王海波,李振国.HPLC波长切换技术同时测定知柏地黄丸(浓缩丸)中莫诺苷、芒果苷、马钱苷和丹皮酚的含量[J].药物分析杂志,2015,35(1):125-128.
[6]潘莹,郭小龙,陈勇,等.HPLC法测定杞菊地黄丸中马钱苷、芍药苷和丹皮酚的含量[J].中国药科大学学报,2007,38(2):133-135.
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[8]李娴,王本杰,袁桂艳,等.六味地黄丸中四种活性成分的HPLC法测定[J].中国医药工业杂志,2010,41(2):126-128.
[9]王晓燕,霍甜甜,李振国,等.一测多评法同时测定杞菊地黄口服液中4种有效成分的含量[J].药物分析杂志,2017,37(2):290-296.
[10]张雪,彭富全,何风雷.一测多评法测定昆仙胶囊中10种黄酮类成分[J].中草药,2018,49(24):5823-5829.
[11]冯兵,陈婷,赵瑞芝,等.HPLC测定复方昆丹胶囊中芍药内酯苷、芍药苷、二苯乙烯苷、五没食子酰葡萄糖[J].中国实验方剂学杂志,2012,18(7):112-116.
[12]韩根利,刘宏胜,王树森,等.RP-HPLC法同时测定山茱萸萜类制剂中莫诺苷、马钱苷、山茱萸新苷、齐墩果酸及熊果酸[J].中草药,2017,48(24):5168-5173.
[13]郑艳萍,朱红军,秦昆明,等.川建曲中5种成分含量的测定及HPLC指纹图谱的初步建立[J].中药材,2018,41(5):1139-1142.
[14]任莹,范姣姣,张鑫.HPLC法测定复方双花片中绿原酸、咖啡酸、连翘苷、穿心莲内酯和木犀草素[J].现代药物与临床,2017,32(7):1192-1195.
[15]李静,张青,肖春霞,等.HPLC波长切换法同时测定排毒养颜胶囊中10种成分[J].中草药,2018,49(20):4824-4830.
[2]陶娜,李亚兰,项奕.杞菊地黄丸对白内障术后干眼症患者疗效,BμT,SIT及FL的影响[J].中国实验方剂学杂志,2017,23(23):166-170.
[3]黎绮雯.杞菊地黄丸联合重组成纤维细胞生长因子凝胶治疗白内障术后干眼症的临床研究[J].中医药导报,2016,22(6):93-95.
[4]中华人民共和国卫生部药品标准.中药成方制剂(第十一册)[S].1996.
[5]李桂本,王海波,李振国.HPLC波长切换技术同时测定知柏地黄丸(浓缩丸)中莫诺苷、芒果苷、马钱苷和丹皮酚的含量[J].药物分析杂志,2015,35(1):125-128.
[6]潘莹,郭小龙,陈勇,等.HPLC法测定杞菊地黄丸中马钱苷、芍药苷和丹皮酚的含量[J].中国药科大学学报,2007,38(2):133-135.
[7]李润泽,常增荣,傅欣彤,等.HPLC法测定杞菊地黄丸中莫诺苷、马钱苷和丹皮酚的含量[J].药物分析杂志,2015,35(2):351-354.
[8]李娴,王本杰,袁桂艳,等.六味地黄丸中四种活性成分的HPLC法测定[J].中国医药工业杂志,2010,41(2):126-128.
[9]王晓燕,霍甜甜,李振国,等.一测多评法同时测定杞菊地黄口服液中4种有效成分的含量[J].药物分析杂志,2017,37(2):290-296.
[10]张雪,彭富全,何风雷.一测多评法测定昆仙胶囊中10种黄酮类成分[J].中草药,2018,49(24):5823-5829.
[11]冯兵,陈婷,赵瑞芝,等.HPLC测定复方昆丹胶囊中芍药内酯苷、芍药苷、二苯乙烯苷、五没食子酰葡萄糖[J].中国实验方剂学杂志,2012,18(7):112-116.
[12]韩根利,刘宏胜,王树森,等.RP-HPLC法同时测定山茱萸萜类制剂中莫诺苷、马钱苷、山茱萸新苷、齐墩果酸及熊果酸[J].中草药,2017,48(24):5168-5173.
[13]郑艳萍,朱红军,秦昆明,等.川建曲中5种成分含量的测定及HPLC指纹图谱的初步建立[J].中药材,2018,41(5):1139-1142.
[14]任莹,范姣姣,张鑫.HPLC法测定复方双花片中绿原酸、咖啡酸、连翘苷、穿心莲内酯和木犀草素[J].现代药物与临床,2017,32(7):1192-1195.
[15]李静,张青,肖春霞,等.HPLC波长切换法同时测定排毒养颜胶囊中10种成分[J].中草药,2018,49(20):4824-4830.
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