药用蜂蜜中5-羟甲基糠醛的限量检查方法研究

目的：研究药用蜂蜜中5-羟甲基糠醛（5-hydroxymethyl furfural，5-HMF）的限量检查方法。方法：采用高效液相色谱法，使用C₁₈色谱柱（4.6 mm×250 mm，5 μm），以乙腈-0.1%甲酸（5：95）为流动相，流速0.8 mL·min^-1，检测波长为284 nm（5-HMF）、254 nm（鸟苷），柱温35℃。采用以鸟苷为内标物，以鸟苷/5-HMF的校正因子计算含量；同时采用外标法测定5-HMF的含量，比较校正因子法计算值与外标法实测值得差异。结果：鸟苷/5-HMF不同浓度比值（0.34~3.46）与峰面积比值的线性关系良好（r=0.999 9），检出限为0.1 ng，加样回收率（n=6）为101.4%（RSD=4.7%）；各批样品中5-HMF的计算值与实测值间无显著差异（P=0.411）。结论：本法可用于药用蜂蜜中5-羟甲基糠醛的限量检查。

Objective:To establish a method for limit test of 5-hydroxymethyl furfural (5-HMF) in medicinal honey.Methods:HPLC with C₁₈ column(4.6 mm×250 mm,5 μm) was adopted,the mobile phase consisted of acetonitrile and 0.1% formic acid solution (5:95) at a flow rate of 0.8 mL·min^-1,the detection wavelengths were 284 nm for 5-HMF and 254 nm for guanosine,the column temperature was 35℃. With guanosine as internal standard,5-HMF was determined by both external standard method and correction factor of 5-HMF/guanosine. The validity of the correction factor method was evaluated by comparison of the quantitative results of both methods. Results:The concentration radio of guanosine to 5-HMF was between 0.34 and 3.46,and the related radio of peaks area revealed a good relationship. The lowest detection limit was 0.1 ng and the average recovery (n=6) was 101.4% (RSD=4.7%).No significant difference was observed between results of external standard method and correction factor method in 21 batches of medicinal honey (P=0.411).Conclusion:The method is feasible for limit test of the medicinal honey.