HPLC测定石榴子中的3种化学成分

Determination of three chemical components in pomegranate seeds by HPLC

目的研究不同干燥温度、干燥时间下石榴子药材中果糖、葡萄糖与5-羟甲基糠醛(5-HMF)含量的变化规律,为评价石榴子质量提供参考。方法取石榴子药材,置60、80、105℃的烘箱中,分别烘1、4、8、12、18、24、36、48 h后取样;采用Mercury NH_(2)色谱柱(250 mm×4.6 mm,5μm),以乙腈-水(70∶30)为流动相,流速0.5 mL·min^(-1),柱温25℃,示差折光检测器测定样品中果糖、葡萄糖的含量;采用Agilent Zorbax SB-C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.1%甲酸溶液(2∶98)为流动相,流速1.0 mL·min^(-1),柱温30℃,检测波长284 nm,测定样品中5-HMF的含量;采用SPSS 26.0软件分析干燥温度、干燥时间与果糖、葡萄糖、5-HMF含量的相关性。结果随干燥温度及干燥时间的增加,石榴子药材中果糖、葡萄糖的含量呈下降趋势,5-HMF的含量呈上升趋势,温度为80、105℃时,变化较为明显;干燥温度、干燥时间与葡萄糖、果糖、5-HMF的含量呈显著相关,其中,葡萄糖、果糖的含量呈负相关,5-HMF的含量呈正相关。结论石榴子药材干燥加工过程中,温度应控制在60℃以内,时间应不超过48 h;所用方法结果准确、重复性好,可为石榴子药材质量标准的制定及质量控制提供参考。

OBJECTIVE To study the changes of fructose,glucose,and 5-hydroxymethylfurfural(5-HMF)contents in pomegranate seeds under different drying temperatures and drying times,and to provide reference for quality evaluation of pomegranate seeds.METHODS Pomegranate medicinal materials were collected and placed in an oven at set temperatures of 60,80,and 105℃.The samples were collected after 1,4,8,12,18,24,36,and 48 h,respectively.The Mercury NH_(2)column(250 mm×4.6 mm,5μm)was used with acetonitrile-water(70∶30)as the mobile phase for elution.The flow rate was 0.5 mL·min^(-1)and the column temperature was 25℃.The content of fructose and glucose in the sample was determined by differential refractive index detector.Agilent Zorbax SB-C18 column(250 mm×4.6 mm,5μm)was used with the mobile phase of acetonitrile-0.1%formic acid(2∶98)at a flow rate of 1.0 mL·min^(-1).The column temperature was 30℃and the detection wavelength was 284 nm.The content of 5-HMF in samples was determined.The correlation between drying temperature,drying time and fructose,glucose,5-HMF content was analyzed by SPSS 26.0 software.RESULTS With the increase of drying temperature and drying time,the contents of fructose and glucose in pomegranate seeds decreased,and the content of 5-hydroxymethylfurfural increased.When the temperature was set at 80℃and 105℃,the change was more obvious.Drying temperature and drying time were significantly correlated with glucose content,fructose content and 5-HMF content.Glucose content and fructose content were negatively correlated,and 5-HMF content was positively correlated.CONCLUSION During the drying process of pomegranate seeds,the temperature should be kept below 60℃,and the time should not exceed 48 h.The method established in this study has been proven to be accurate and reproducible,which can provide reference for the formulation of quality standards and production quality control of pomegranate seeds.