市售二至丸的UPLC指纹图谱和模式识别分析不同品牌差异研究
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摘要
目的 建立14批市售二至丸的指纹图谱,比较不同品牌二至丸的质量差异。方法 Waters HSS T3(100x1.0mm,1.8μm),流动相A:0.1%甲酸水溶液,流动相B:0.1%甲酸乙腈,波长270nm,柱温25℃,流速0.20ml/min,梯度洗脱(0～1min:80%A;1～20min 65%A;20～22.5min 30%A;22.5～28min 10%A;,28～30min 80%A;30～32min 80%A)。采用主成分分析(PCA)和最小二乘法-判别分析(PLS-DA),观察整体分布趋势和寻找不同品牌的差异峰。结果 14批次市售二至丸建立指纹图谱,共发现20个共有峰,相似度0.95～1.00。同一企业生产FH和HJY品牌样品接近,与另一企业企业LYS品牌距离较远。LYS与FH、HJY的二至丸PLS-DA模型合理,预测性强,二者差异主要体现在特女贞苷和蒙花苷。结论 指纹图谱方法稳定性、精密度和重复符合中药指纹图谱的技术要求,能客观反映市售二至丸的质量。
Objective To establish the fingerprint of Er-Zhi-Wan(EZW) and compare the differences of EZW from different brands. Methods UPLC-DAD method, Chromatographic column: Waters HSS T3(100 x1.0 mm, 1.8 um), mobile phase A: 0.1% formic acid aqueous solution, mobile phase B: 0.1% acetonitrile formic acid, wavelength 270 nm, column temperature 25℃, flow rate 0.20 ml/min, gradient elution(0-1 min: 80% A; 1-20 min: 65% A; 20-22.5 min 30% A; 22.5-28 min: 10% A; 28-30 min: 80% A; 30-32: 80% A). Principal component analysis(PCA) and least squares discriminant analysis(PLSDA) were used to observe the overall distribution trend and find the difference peaks of EZW from different brands. Results Twenty common peaks were found in 14 batches of EZW, 1 from Eclipta herba, 11 from Ligustrum lucidum, 8 from both drugs. It was found that the sample of FH and HJY in same company was close to that of LYS made by another company. The PLS-DA model of FH, HJY and LYS is reasonable and predictive, and the difference between them is mainly reflected in Ligustrin and mononoside. Conclusion The stability, precision and repetition of the fingerprint met the technical requirements of the fingerprint. The similarity of 14 batches of EZW before 0.95-1.00 could objectively reflect the quality of EZW.
Objective To establish the fingerprint of Er-Zhi-Wan(EZW) and compare the differences of EZW from different brands. Methods UPLC-DAD method, Chromatographic column: Waters HSS T3(100 x1.0 mm, 1.8 um), mobile phase A: 0.1% formic acid aqueous solution, mobile phase B: 0.1% acetonitrile formic acid, wavelength 270 nm, column temperature 25℃, flow rate 0.20 ml/min, gradient elution(0-1 min: 80% A; 1-20 min: 65% A; 20-22.5 min 30% A; 22.5-28 min: 10% A; 28-30 min: 80% A; 30-32: 80% A). Principal component analysis(PCA) and least squares discriminant analysis(PLSDA) were used to observe the overall distribution trend and find the difference peaks of EZW from different brands. Results Twenty common peaks were found in 14 batches of EZW, 1 from Eclipta herba, 11 from Ligustrum lucidum, 8 from both drugs. It was found that the sample of FH and HJY in same company was close to that of LYS made by another company. The PLS-DA model of FH, HJY and LYS is reasonable and predictive, and the difference between them is mainly reflected in Ligustrin and mononoside. Conclusion The stability, precision and repetition of the fingerprint met the technical requirements of the fingerprint. The similarity of 14 batches of EZW before 0.95-1.00 could objectively reflect the quality of EZW.
引文
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[2] 国家药典委员会.中国药典:一部[S].北京:中国医药科技出版社,2015:437.
[3] He ZD,Dong H,Xu HX,et al.Secoiridoid constituents from the fruits of Ligustrum lucidum[J].Phytochemistry,2001,56(14):327.
[4] Liu HX,Shi YH,Wang DX,et al.MECC determination of oleanolic acid and ursolic acid isomers in Ligustrum lucidum Ait[J].J Pharm Biomed Anal,2003,32(3),479,
[5] Lee MK,Ha NR,Yang H,et al.Antiproliferative activity of triterpenoids from Eclipta prostratra on hepatic stellate cells[J].Phtomedicine,2008,15(9):775.
[6] Lee MK,Ha NR,Yang H,et al,Stimulatory Constituents of Eclipta prostratra on mouse osteoblast differentiation[J].Phytother Res,2009,23(1):129.
[7] 吴岩斌,林雄浩,吴建国,等.二至丸提取物的HPLC指纹图谱[J].康复学报,2012,22(5):32.
[8] 范妙璇,谭成,王萌萌,等.基于5种特征性成分综合评价二至丸的质量[J].中国实验方剂学杂志 ,2018,24(17):88.
[9] 何睦,姚卫峰,张丽,等.高效液相色谱法同时测定二至丸中4种成分的含量[J].中国中药杂志,2012,37(5):594.
[10] 刘菊,白明学,张红伟,等.反相高效液相色谱法测定二至丸中特女贞苷的含量[J].中南药学,2016,121(2):194.