[关键词]
[摘要]
目的 建立西藏木瓜的HPLC多指标定量指纹图谱,为西藏木瓜的质量控制和真伪鉴别提供方法和技术支持。方法 采用高剪切分散乳化(HSDE)法提取木瓜鲜样,采用Agilent Zorbax SB-C18(250 mm×4.6 mm,5.0μm)色谱柱,乙腈-0.5%冰乙酸+10 mmol/L乙酸铵水溶液为流动相,进行梯度洗脱,体积流量为0.8 mL/min,柱温为25℃,检测波长为280 nm。利用ESI-TOF/MS法对西藏木瓜提取物中多种化合物进行鉴别,在对多指标活性成分进行定量测定的基础上,建立西藏木瓜的HPLC指纹图谱。结果 西藏木瓜HPLC指纹图谱共有30个共有峰,指认了其中9个峰,分别为绿原酸、香草酸、咖啡酸、藜芦酸、芸香苷、槲皮苷、金丝桃苷、齐墩果酸和熊果酸,并对其进行了定量测定。指纹图谱中相似度分析表明,10批西藏木瓜的相似度较为接近,而西藏木瓜与其他品种木瓜的相似度差别较大。结论 HSDE-HPLC-DAD-ESI-TOF/MS法可以用于木瓜鲜样的快速提取和分析,在此基础上建立的指纹图谱结合相似度分析可用于其质量评价,为提高西藏木瓜的质量控制水平提供了方法和技术支持。
[Key word]
[Abstract]
Objective To establish a HSDE-HPLC-DAD-ESI-TOF/MS method for the rapid identification of chemical ingredients for Chaenomeles thibetica, and establish the multi-component quantitative fingerprint to evaluate its quality.Methods The separation was developed via an Agilent Zorbax SB-C18 column (250 mm×4.6 mm, 5.0 μm) with a gradient elution at a temperature of 25℃, the acetonitrile was used as the mobile phase A and 0.5% glacial acetic acid and 10 mM ammonium acetate solution was used as the mobile phase B with a flow rate of 0.8 mL/min, and the detection wavelength was 280 nm. ESI-TOF/MS was used for the identification of chemical ingredients in C. thibetica. The fingerprint of C. thibetica was established based on the quantitative detection of multi-components.Results The HPLC fingerprint of C. thibetica has 30 common peaks, nine ingredients (chlorogenic acid, vanillic acid, caffeic acid, veratric acid, rutin, quercitrin, hyperin, oleanolic acid, and uosolic acid) of C. thibetica were identified, and the contents of them were determined. Similarity analysis shows that the similarity of 10 batches of C. thibetica is relatively close, while the similarity between C. thibetica and other varieties' is quite different.Conclusion HSDE-HPLC-DAD-ESI-TOF/MS method can be used for the rapid extraction and analysis of C. thibetica fresh samples. On this basis, the fingerprint analysis combined with similarity analysis can be used for quality evaluation of C. thibetica.
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[基金项目]
山东省自然科学基金资助项目(ZR2013HL029,ZR2017LH071);山东省科技发展计划(2016GSF202014);山东省泰山学者岗位资助项目;山东省科学院先导专项