HPLC法同时测定肝炎康散中四种有效成分及指纹图谱研究
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摘要
目的本文旨在HPLC条件下建立一种同时测定肝炎康散中四种成分含量并建立其在该波长下的指纹图谱的方法。方法采用高效液相色谱法,Universil XB C_(18)色谱柱(150 mm×2.1 mm,1.8μm),流动相:水(A)-乙腈(B),梯度洗脱,流速1.0 mL·min~(-1),检测波长280 nm,进样量30μL,柱温为30℃;建立肝炎康散指纹图谱,运用中国药典委员会"中药色谱指纹图谱相似度评价系统软件"对10批制剂进行相似度评价,并对其中4个色谱峰进行指认,同时测定虎杖苷、五味子醇甲、白术内酯I、白术内酯II四种有效成分的含量。结果 10批肝炎康散指纹图谱中标定了14个共有色谱峰,相似度值为0.990～0.998。虎杖苷、五味子醇甲、白术内酯I、白术内酯II质量浓度分别在12.2～73.4 mg·L~(-1)、60.1～360.5 mg·L~(-1)、59.8～361.0 mg·L~(-1)、60.2～361.0 mg·L~(-1)内,与峰面积呈良好的线性关系,平均回收率分别为98.5%、99.0%、97.6%、99.1%,RSD为1.2%、1.9%、1.6%、1.1%(n=6)。结论建立的肝炎康散的指纹图谱结合有关成分含量测定,具有实际应用意义,能更好的对肝炎康散进行质量控制。
Objective Aim To establish a method for the simultaneous determination of four components in Ganyankang San and the establishment of its fingerprint at this wavelength under HPLC conditions.Methods High performance liquid chromatography(HPLC)was used on a Universil XB C_(18) column(150 mm×2.1 mm,1.8 μm)with a mobile phase of water(A)-acetonitrile(B),gradient elution at a flow rate of 1 mL·min~(-1),the injection volume was 30 μL and the column temperature was 30 ℃.The Ganyankang San fingerprinting was established and the similarity of 10 batches of preparations was evaluated by the Chinese Pharmacopoeia Commission′s "Software for Similarity Evaluation of Chromatographic Fingerprints of Traditional Chinese Medicines" Chromatographic peaks were identified and determination of content,while measuring polydatin,Schisandra alcohol A,atractylodes I,atractylodes lactone II.Results Ten batches of Ganyankang San fingerprints were calibrated for 14 common peaks with the similarities of 0.990～0.998.The concentrations of polydatin,schisandrin,atractylodes I and atractyloside II were 12.2-73.4 mg·L~(-1),60.1-360.5 mg·L~(-1),59.8-361.0 mg·L~(-1),60.2-361.0 mg·L~(-1),the average recoveries were 98.5%,99.0%,97.6%,99.1%,RSD 1.2%,1.9%,1.6%,1.1%.Conclusion The established Ganyankang San fingerprinting method combined with the determination of related components has practical significance,which can better control the quality of Ganyankang San.
Objective Aim To establish a method for the simultaneous determination of four components in Ganyankang San and the establishment of its fingerprint at this wavelength under HPLC conditions.Methods High performance liquid chromatography(HPLC)was used on a Universil XB C_(18) column(150 mm×2.1 mm,1.8 μm)with a mobile phase of water(A)-acetonitrile(B),gradient elution at a flow rate of 1 mL·min~(-1),the injection volume was 30 μL and the column temperature was 30 ℃.The Ganyankang San fingerprinting was established and the similarity of 10 batches of preparations was evaluated by the Chinese Pharmacopoeia Commission′s "Software for Similarity Evaluation of Chromatographic Fingerprints of Traditional Chinese Medicines" Chromatographic peaks were identified and determination of content,while measuring polydatin,Schisandra alcohol A,atractylodes I,atractylodes lactone II.Results Ten batches of Ganyankang San fingerprints were calibrated for 14 common peaks with the similarities of 0.990～0.998.The concentrations of polydatin,schisandrin,atractylodes I and atractyloside II were 12.2-73.4 mg·L~(-1),60.1-360.5 mg·L~(-1),59.8-361.0 mg·L~(-1),60.2-361.0 mg·L~(-1),the average recoveries were 98.5%,99.0%,97.6%,99.1%,RSD 1.2%,1.9%,1.6%,1.1%.Conclusion The established Ganyankang San fingerprinting method combined with the determination of related components has practical significance,which can better control the quality of Ganyankang San.
引文
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[9] 赵萍,王森,欧水平,等.HPLC法同时测定虎杖膏中4种成分的含量[J].中国药房,2017,28(3):405-407.
[2] 李斌.护肝颗粒中五味子醇甲含量测定方法研究[J].黑龙江医药,2014(1):27-29.
[3] 杨立志,姜雪敏.高效液相色谱法测定利肺片中五味子醇甲、五味子甲素及五味子乙素含量[J].中国药业,2017,26(2):38-40.
[4] 李羾,何丹,杨常成.高效液相色谱法测定白术中白术内酯Ⅰ、Ⅱ和Ⅲ的含量[J].中南药学,2014(1):70-73.
[5] 刘芷,贾英,赵旭,等.五味子的UPLC指纹图谱研究[J].中草药,2014,45(11):1631-1633.
[6] 唐德智.HPLC法测定复方黄芩片中6个成分的含量[J].药物分析杂志,2016,36(10):1870-1874.
[7] 谢健鸣,隆颖.HPLC法同时测定补正片中虎杖苷、补骨脂素及异补骨脂素的含量[J].中国医药科学,2016,6(9):32-35.
[8] 蒋叔霏.虎梅颗粒中薄荷脑薄层色谱鉴别与虎杖苷含量测定[J].中国药业,2013,22(19):43-45.
[9] 赵萍,王森,欧水平,等.HPLC法同时测定虎杖膏中4种成分的含量[J].中国药房,2017,28(3):405-407.