摘要
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C_(18)色谱柱(4.6 mm×250 mm,5μm),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 C_(18) 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 m L·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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第2期326-330,共5页
Chinese Journal of Pharmaceutical Analysis