麦冬与山麦冬中多元指标成分的比较分析
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摘要
建立超快速液相色谱-三重四级杆/线性离子阱质谱(UFLC-QTRAP-MS/MS)同时测定麦冬类药材中甾体皂苷、高异黄酮、氨基酸与核苷类共33种指标成分含量测定的方法,并结合多元统计分析对麦冬类商品药材进行比较分析。采用SynergiTMHydro-RP 100(2. 0 mm×100 mm,2. 5μm)色谱柱,以0. 1%甲酸水-0. 1%甲酸乙腈为流动相,流速0. 4 mL·min~(-1),梯度洗脱,多反应监测模式检测(MRM);用聚类分析(HCA)、主成分分析(PCA)和偏最小二乘判别分析(PLS-DA)进行数据处理和分析。结果显示,33种目标成分在一定浓度范围内线性关系良好(r> 0. 999 0);加样回收率为96. 23%~102. 0%,RSD均小于5. 0%。麦冬与山麦冬化学成分差异明显,找出7种差异显著的化学成分。该研究为麦冬类药材内在质量的综合评价和全面控制提供依据,同时为麦冬与山麦冬的药材鉴别提供新的方法参考。
An analytical method based on UFLC-QTRAP-MS/MS was established for simultaneous determination of thirty-three components including steroidal saponins,homoisoflavonoids,amino acids and nucleosides in Ophiopogonis Radix. Thirty-three target components of commercial medicinal materials of Maidong were comparative analysis. SynergiTMHydro-RP 100 column(2. 0 mm ×100 mm,2. 5 μm) was used with 0. 1% formic acid solution-0. 1% formic acid acetonitrile for gradient elution at a flow rate of 0. 4 mL·min~(-1). In addition,multiple reaction monitoring(MRM) mode was employed. The data were comprehensively processed and analyzed with hierarchical clustering analysis(HCA),principal component analysis(PCA) and partial least squares discriminant analysis(PLS-DA) methods. All components showed good linearity(r > 0. 999 0) within the tested ranges. The average recoveries were between 96. 23%-102. 0%,and the relative standard deviation(RSD) were less than 5%. The results showed that there were significant differences in components between Ophiopogonis Radix and Liriopes Radix,with seven components obviously different. This method was useful for providing basis for the comprehensive evaluation and intrinsic quality control of Ophiopogonis Radix and Liriopes Radix,and may provide a new method reference for the identification of Ophiopogonis Radix and Liriopes Radix.
An analytical method based on UFLC-QTRAP-MS/MS was established for simultaneous determination of thirty-three components including steroidal saponins,homoisoflavonoids,amino acids and nucleosides in Ophiopogonis Radix. Thirty-three target components of commercial medicinal materials of Maidong were comparative analysis. SynergiTMHydro-RP 100 column(2. 0 mm ×100 mm,2. 5 μm) was used with 0. 1% formic acid solution-0. 1% formic acid acetonitrile for gradient elution at a flow rate of 0. 4 mL·min~(-1). In addition,multiple reaction monitoring(MRM) mode was employed. The data were comprehensively processed and analyzed with hierarchical clustering analysis(HCA),principal component analysis(PCA) and partial least squares discriminant analysis(PLS-DA) methods. All components showed good linearity(r > 0. 999 0) within the tested ranges. The average recoveries were between 96. 23%-102. 0%,and the relative standard deviation(RSD) were less than 5%. The results showed that there were significant differences in components between Ophiopogonis Radix and Liriopes Radix,with seven components obviously different. This method was useful for providing basis for the comprehensive evaluation and intrinsic quality control of Ophiopogonis Radix and Liriopes Radix,and may provide a new method reference for the identification of Ophiopogonis Radix and Liriopes Radix.
引文
[1]中国药典.一部[S]. 2015:155.
[2]刘治民,胡光华,孙冶,等.吉林省流通麦冬质量评价研究[J].中国现代中药,2017,19(1):73.
[3]殷晓华.麦冬及其类似品、伪品的鉴别[J].中草药,2000(4):65.
[4]王磊,秦玖刚,王川.麦冬提取物对胰岛素抵抗大鼠肝组织miRNA-29a及FOXO3表达的影响[J].中国实验方剂学杂志,2018,24(1):124.
[5]Chen M H,Chen X J,Wang M,et al. Ophiopogon japonicus-A phytochemical,ethnomedicinal and pharmacological review[J]. J Ethnopharmacol,2016(181):193.
[6]晏仁义,马凤霞,余河水,等. UPLC-Q-TOF-MSE结合相对保留时间在线快速鉴定麦冬中甾体皂苷类成分[J].中国实验方剂学杂志,2016,22(24):43.
[7]李正,陈勇,马临科,等.浙麦冬质量标准的制定及探讨[J].中国现代应用药学,2016,33(6):795.
[8]吴发明,蔡晓洋,王盼,等. HPLC同时测定麦冬中5个皂苷成分的含量[J].中国中药杂志,2015,40(20):4022.
[9]王杰,熊爱珍,程绒绒,等.不同来源引流熊胆粉的化学成分系统分析[J].中国中药杂志,2018,43(11):2326.
[10]吴发明,张思荻,曾俊,等. HPLC-ELSD法测定不同产地麦冬中4种代表性成分的含量[J].药物分析杂志,2016(8):1370.
[11]Wu Y,Dong Z,Wu H,et al. Comparative studies on Ophiopogonis and Liriopes based on the determination of 11 bioactive components using LC-MS/MS and hierarchical clustering analysis[J]. Food Res Int,2014,57(1):15.
[12]韩凤梅,李紫,张玲,等.山麦冬和麦冬皂苷类成分的HPLC/ESI-MS图谱研究[J].中国药学杂志,2005(21):23.
[13]陈勇,李紫,蔡敏.山麦冬、麦冬对照药材电喷雾-质谱(ESIMS)特征图谱的比较研究[J].分析科学学报,2004(2):117.
[2]刘治民,胡光华,孙冶,等.吉林省流通麦冬质量评价研究[J].中国现代中药,2017,19(1):73.
[3]殷晓华.麦冬及其类似品、伪品的鉴别[J].中草药,2000(4):65.
[4]王磊,秦玖刚,王川.麦冬提取物对胰岛素抵抗大鼠肝组织miRNA-29a及FOXO3表达的影响[J].中国实验方剂学杂志,2018,24(1):124.
[5]Chen M H,Chen X J,Wang M,et al. Ophiopogon japonicus-A phytochemical,ethnomedicinal and pharmacological review[J]. J Ethnopharmacol,2016(181):193.
[6]晏仁义,马凤霞,余河水,等. UPLC-Q-TOF-MSE结合相对保留时间在线快速鉴定麦冬中甾体皂苷类成分[J].中国实验方剂学杂志,2016,22(24):43.
[7]李正,陈勇,马临科,等.浙麦冬质量标准的制定及探讨[J].中国现代应用药学,2016,33(6):795.
[8]吴发明,蔡晓洋,王盼,等. HPLC同时测定麦冬中5个皂苷成分的含量[J].中国中药杂志,2015,40(20):4022.
[9]王杰,熊爱珍,程绒绒,等.不同来源引流熊胆粉的化学成分系统分析[J].中国中药杂志,2018,43(11):2326.
[10]吴发明,张思荻,曾俊,等. HPLC-ELSD法测定不同产地麦冬中4种代表性成分的含量[J].药物分析杂志,2016(8):1370.
[11]Wu Y,Dong Z,Wu H,et al. Comparative studies on Ophiopogonis and Liriopes based on the determination of 11 bioactive components using LC-MS/MS and hierarchical clustering analysis[J]. Food Res Int,2014,57(1):15.
[12]韩凤梅,李紫,张玲,等.山麦冬和麦冬皂苷类成分的HPLC/ESI-MS图谱研究[J].中国药学杂志,2005(21):23.
[13]陈勇,李紫,蔡敏.山麦冬、麦冬对照药材电喷雾-质谱(ESIMS)特征图谱的比较研究[J].分析科学学报,2004(2):117.