用反相高效液相色谱-紫外检测法测定1-脱氧野尻霉素的含量

Determination of 1-deoxynojirimycin Content by Ultraviolet Reversed-phase High Performance Liquid Chromatography

以0.05 mol/L HC l为溶剂提取蚕粉和桑叶粉中的1-脱氧野尻霉素(DNJ),并用9-芴基氯甲酸甲酯(FMOC)为衍化剂,在pH 8.5的硼酸盐缓冲液中进行衍生化反应,生成具有紫外吸收的DNJ-FMOC络合物,再用反相高效液相色谱-紫外检测法对其分离测定。结果表明,反应产物的色谱图分离效果良好,DNJ-FMOC的峰面积与DNJ浓度呈高度正相关关系,加样回收率平均为100.7%。精密度试验、稳定性试验、重现性试验、回收率试验表明,该方法稳定可靠,可以作为测定家蚕、桑叶及有关药物样品中DNJ含量的有效方法。

In this experiment, 1-deoxynojirimycin （DNJ） in the silkworm larvae powder and mulberry leaf powder was extracted with 0.05 mol/L HCl, then it was derived by 9-fluorenylmethyl （FMOC） in pH 8.5 borate buffer solution. DNJ-FMOC came into being complex compound, which can be detected by ultraviolet. We separated and detected it by UV-RP-HPLC. The result indicated that the product was separated entirely. There are the most positive relevance between the peak area of DNJ-FMOC and the concentration of DNJ. The average recovery ratio of adding sample is 100, 7%. The precision experiment, stability experiment, repeatability experiment and recovery rate experiment showed that the method is credible, so it can be used as an efficient method to detect DNJ content in the silkworm, mulberry and some other related medicines.