中国中药杂志

2019, v.44(14) 3070-3077

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基于HPLC波长切换法测定7种成分和化学计量学的苏合香质量评价研究
Quality evaluation of Styrax based on quantitative determination of 7 chemical components using HPLC wavelength switching method and chemometrics

黄晓婧;李婷婷;肖春霞;许莉;张定堃;文永盛;谭鹏;
HUANG Xiao-jing;LI Ting-ting;XIAO Chun-xia;XU Li;ZHANG Ding-kun;WEN Yong-sheng;TAN Peng;Chengdu Institute for Food and Drug Control;College of Pharmacy,Chengdu University of Traditional Chinese Medicine;

摘要(Abstract):

为了更全面地评价苏合香的质量,该文尝试建立一种HPLC波长切换法同时测定苏合香中7种成分的含量,通过化学计量学分析不同来源苏合香的质量差异,最终建立苏合香的色谱特征图谱。色谱柱为Agilent ZORBAX Extend C18(4. 6 mm×250 mm,5μm),流动相为乙腈-0. 1%磷酸水溶液,梯度洗脱,检测波长为:0~13. 5 min,194 nm(苯甲酸); 13. 5~20. 5 min,278 nm(肉桂酸); 20. 5~32 min,194 nm(苯甲酸苄酯、肉桂酸苄酯、肉桂酸肉桂酯、脱氢松香酸); 32~55 min,241 nm(松香酸)。方法学验证结果显示苯甲酸、肉桂酸、苯甲酸苄酯、肉桂酸苄酯、肉桂酸肉桂酯、脱氢松香酸、松香酸的进样质量分别在0. 006 948~0. 694 8,0. 001 426~0. 142 6,0. 013 16~0. 658 0,0. 006 148~0. 614 8,0. 008 035~0. 803 5,0. 002 121~0. 212 1,0. 010 172~1. 017 2μg与峰面积呈良好的线性关系,平均加样回收率在94. 34%~105. 8%,RSD均小于3. 0%(n=6)。方法学验证结果表明该文建立的HPLC波长切换法具有较好的准确性、重复性。样品测定结果显示不同来源的苏合香药材质量差异较大。以中国食品药品检定研究院提供的苏合香对照药材(S1)的色谱图为参照谱图,计算各批次样品的指纹图谱相似性。结果显示,S2~S10的相似度分别为0. 952,0. 949,0. 981,0. 351,0. 751,0. 969,0. 979,0. 992,0. 971,0. 971,除S5,S6药材的相似度差异较大外,其他批次的供试品的相似度较好,表明其质量差异较小; S11~S20的相似度分别为0. 060,0. 055,0. 054,0. 285,0. 092,0. 002,0. 044,0. 044,0. 044,0. 040,结果表明S11~S20与对照药材相比,整体质量差异较大。以S1~S10的色谱图为基础,建立了苏合香的HPLC特征图谱,供其他药学研究者参考。该文建立的含量测定方法及特征图谱分析方法简便、重复性好、专属性强,为苏合香的整体质量评控提供了一种参考方法。
In order to evaluate the quality of Styrax more comprehensively,this study attempted to establish an HPLC wavelength switching method to simultaneously determine the content of seven compounds in Styrax,and chemometrics were used to analyze the quality difference between different sources of Styrax,and finally establish a characteristic chromatogram of Styrax. The column was Agilent ZORBAX Extend C18( 4. 6 mm×250 mm,5 μm) with phase a mixture of acetonitrile-0. 1% phosphoric acid aqueous solution as the mobile phase in a gradient elution procedure; the detection wavelength was set as follows: 0-13. 5 min,194 nm( benzoic acid);13. 5-20. 5 min,278 nm( cinnamic acid); 20. 5-32 min,194 nm( benzyl benzoate,benzyl cinnamate,cinnamyl cinnamate,dehydroabietic acid); 32-55 min,241 nm( abietic acid). The methodological verification results showed that when the injection masses of benzoic acid,cinnamic acid,benzyl benzoate,benzyl cinnamate,cinnamyl cinnamate,dehydroabietic acid and abietic acid were0. 006 948-0. 694 8,0. 001 426-0. 142 6,0. 013 16-0. 658 0,0. 006 148-0. 614 8,0. 008 035-0. 803 5,0. 002 121-0. 212 1,and0. 010 172-1. 017 2 μg,respectively,there were good linear relationship between injection mass and peak area. The average recovery rates of seven compounds were in the range from 94. 34% to 105. 8%,and all RSD were less than 3. 0%( n = 6). The methodological verification results showed that the developed HPLC wavelength switching method has good accuracy and repeatability. The results of the sample analysis showed that the quality of Styrax from different sources was quite different. The chromatogram of Styrax reference material( S1) was used as the reference chromatogram to calculate the fingerprint similarity of each batch of samples. The results showed that the similarities of samples S2-S10 were 0. 952,0. 949,0. 981,0. 351,0. 751,0. 969,0. 979,0. 992 and 0. 971,respectively.The similarity values of other batches samples were satisfactory,except for sample S5 and S6,indicating that the quality difference among these samples is small. The similarity values of S11-S20 were 0. 060,0. 055,0. 054,0. 285,0. 092,0. 002,0. 044,0. 044,0. 044,and 0. 040,respectively. The results showed that compared with the sample S1,there was a large quality difference among S11-S20. Based on the chromatograms of S1-S10,the HPLC characteristic chromatograms of Styrax was established and the purpose is to give reference to other pharmaceutical researchers. The newly developed HPLC wavelength switching method have the advantages of simplicity,reproducibility and specificity,and the developed HPLC characteristic chromatograms provided a reference method for the overall quality evaluation of Styrax.

关键词(KeyWords): 苏合香;HPLC;波长切换法;化学计量学;指纹图谱;质量评价
Styrax;HPLC;wavelength switching;chemometrics;fingerprint chromatogram;quality evaluation

Abstract:

Keywords:

基金项目(Foundation): 国家自然科学基金项目(81873232);; 四川省科技厅应用基础研究项目(2019YJ0640);; 成都市科技局技术创新研发项目(2018-YF05-01277-SN);成都市科技局科技惠民项目(2016-HM01-00312-SF)

作者(Author): 黄晓婧;李婷婷;肖春霞;许莉;张定堃;文永盛;谭鹏;
HUANG Xiao-jing;LI Ting-ting;XIAO Chun-xia;XU Li;ZHANG Ding-kun;WEN Yong-sheng;TAN Peng;Chengdu Institute for Food and Drug Control;College of Pharmacy,Chengdu University of Traditional Chinese Medicine;

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DOI: 10.19540/j.cnki.cjcmm.20190423.201

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