甘草微型饮片切制工艺及UPLC指纹图谱
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摘要
目的优化甘草微型饮片切制工艺,建立其UPLC指纹图谱。方法以流动性、出膏率以及甘草苷、甘草酸、甘草素、甘草次酸、异甘草素、查耳酮含有量为评价指标,软化时间、饮片厚度、饮片粒径、干燥温度为影响因素,正交试验优化切制工艺。甘草70%乙醇提取物的分析采用BEH C_(18)色谱柱(2. 1 mm×50 mm,1. 7μm);流动相乙腈-0. 1%磷酸,梯度洗脱;体积流量0. 3 mL/min;柱温25℃;检测波长237 nm。结果最佳工艺为粒径0. 5～0. 9 mm,厚度1 mm,软化时间1 h,干燥温度50℃。10批样品UPLC指纹图谱中有25个共有峰,相似度均大于0. 9。6种成分在各自范围内线性关系良好(R~2>0. 999 0),平均加样回收率为99. 4%～102. 5%,RSD 0. 29%～1. 9%。结论该方法准确稳定,重复性好,可用于甘草微型饮片的质量控制。
AIM To optimize the cutting process and to establish UPLC fingerprints of Glycyrrhiza uralensis Fisch mini slices. METHODS With flowing time,leaching rate and the contents of glycyrrhizin,glycyrrhizin,glycyrrhizin,glycyrrhetinic acid,isoliquiritigenin,chalcone as evaluation indices,soften time,pieces thickness,pieces diameter and drying temperature as influencing factors,the cutting process was optimized by orthogonal test.The analysis of 70% ethanol extract of G. uralensis was performed on a 25 ℃ thermostatic BEH C_(18)column( 2. 1mm× 50 mm,1. 7 μm),with the mobile phase comprising of acetonitrile-0. 1% phosphoric acid flowing at 0. 3mL/min in a gradient elution manner,and the detection wavelength was set at 237 nm. RESULTS The optimal cutting process conditions were determined to be 0. 5-0. 9 mm for the grain size,1 mm for the thickness,1 h for the soften time,and 50 ℃ for the drying temperature. There were twenty-five common peaks in the UPLC fingeprints of ten batches of samples with the similarities of more than 0. 9. Six constituents showed good linear relationships within their own ranges( R~2> 0. 999 0),whose average recoveries were 99. 4%-102. 5% with the RSDs of0. 29%-1. 9%. CONCLUSION This accurate,stable and reproducible method can be used for the quality control of G. uralensis mini slices.
AIM To optimize the cutting process and to establish UPLC fingerprints of Glycyrrhiza uralensis Fisch mini slices. METHODS With flowing time,leaching rate and the contents of glycyrrhizin,glycyrrhizin,glycyrrhizin,glycyrrhetinic acid,isoliquiritigenin,chalcone as evaluation indices,soften time,pieces thickness,pieces diameter and drying temperature as influencing factors,the cutting process was optimized by orthogonal test.The analysis of 70% ethanol extract of G. uralensis was performed on a 25 ℃ thermostatic BEH C_(18)column( 2. 1mm× 50 mm,1. 7 μm),with the mobile phase comprising of acetonitrile-0. 1% phosphoric acid flowing at 0. 3mL/min in a gradient elution manner,and the detection wavelength was set at 237 nm. RESULTS The optimal cutting process conditions were determined to be 0. 5-0. 9 mm for the grain size,1 mm for the thickness,1 h for the soften time,and 50 ℃ for the drying temperature. There were twenty-five common peaks in the UPLC fingeprints of ten batches of samples with the similarities of more than 0. 9. Six constituents showed good linear relationships within their own ranges( R~2> 0. 999 0),whose average recoveries were 99. 4%-102. 5% with the RSDs of0. 29%-1. 9%. CONCLUSION This accurate,stable and reproducible method can be used for the quality control of G. uralensis mini slices.
引文
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[12]孙玉雯,刘起华,程艳玲,等.中药煮散与传统饮片煎煮效率的对比研究-皮类、茎木类及果实种子类药材[J].西北药学杂志,2016,31(4):337-341.
[13]段天璇,于密密,刘春生,等. HPLC法同时测定甘草指纹图谱暨甘草苷、甘草酸含量[J].中成药,2006,28(2):161-165.
[14]苏本正,周倩,孙立立.甘草饮片乙酸乙酯提取部位HPLC指纹图谱研究[J].中成药,2011,33(2):203-207.
[15]周倩,戴衍朋,王亮,等. HPLC法测定生甘草、炙甘草中6种成分[J].中成药,2016,38(2):378-382.
[16]李强,杜思邈,张忠亮,等.中药指纹图谱技术进展及未来发展方向展望[J].中草药, 2013, 44(22):3095-3104.
[17]吴昭晖,罗佳波,游文玮.甘草药材HPLC指纹图谱研究[J].中草药,2005,36(12):1868-1872.
[18]赵义.水泥粉体流动性能的研究[J].山东建材,2000(3):12-13.
[2]胡金锋,沈凤嘉.甘草属植物化学成分研究概况[J].天然产物研究与开发,1996,8(3):77-91.
[3]田庆来,官月平,张波,等.甘草有效成分的药理作用研究进展[J].天然产物研究与开发,2006,18:343-347.
[4] Zhang Q,Ye M. Chemical analysis of the Chinese herbal medicine Gan-Cao(licorice)[J]. J Chromatogr A,2009,1216(11):1954-1969.
[5] Hatano T,Takagi M,Ito H,et al. Acylated flavonoid glycosides and accompanying phenolics from licorice[J]. Phytochemistry,1998,47(2):287-293.
[6]苏苗,张晶,尤艳艳,等.不同产地甘草有效成分含量分析[J].中南药学,2014,12(10):1022-1024.
[7]黄明进,王文全,魏胜利.我国甘草药用植物资源调查及质量评价研究[J].中国中药杂志, 2010, 35(8):947-952.
[8]林桂梅,张天连,贾天柱.枳实、枳壳微型饮片切制工艺优化[J].中成药,2017,39(11):2396-2400.
[9]孙磊,乔善义,赵毅民.中药指纹图谱应用研究进展[J].国际药学研究杂志,2009,36(3):194-197,203.
[10]林俊芝,傅超美,毛茜,等.黄柏饮片与煮散颗粒在不同煎煮时间点盐酸小檗碱含量和干膏收率的比较[J].中国实验方剂学杂志,2012,18(12):41-43.
[11]舒波,龙阳,李毅.粒度对大黄饮片(药材)有效成分的影响分析[J].医学信息,2015(38):18-19.
[12]孙玉雯,刘起华,程艳玲,等.中药煮散与传统饮片煎煮效率的对比研究-皮类、茎木类及果实种子类药材[J].西北药学杂志,2016,31(4):337-341.
[13]段天璇,于密密,刘春生,等. HPLC法同时测定甘草指纹图谱暨甘草苷、甘草酸含量[J].中成药,2006,28(2):161-165.
[14]苏本正,周倩,孙立立.甘草饮片乙酸乙酯提取部位HPLC指纹图谱研究[J].中成药,2011,33(2):203-207.
[15]周倩,戴衍朋,王亮,等. HPLC法测定生甘草、炙甘草中6种成分[J].中成药,2016,38(2):378-382.
[16]李强,杜思邈,张忠亮,等.中药指纹图谱技术进展及未来发展方向展望[J].中草药, 2013, 44(22):3095-3104.
[17]吴昭晖,罗佳波,游文玮.甘草药材HPLC指纹图谱研究[J].中草药,2005,36(12):1868-1872.
[18]赵义.水泥粉体流动性能的研究[J].山东建材,2000(3):12-13.