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作 者:陈蓓[1] 李放[1] 刘华良[1] 吉文亮[1] CHEN Bei;LI Fang;LIU Hua-Liang;JI Wen-Liang(Jiangsu Provincial Center for Disease Control and Prevention,Nanjing 210009,China)
出 处:《食品安全质量检测学报》2018年第22期5877-5880,共4页Journal of Food Safety and Quality
基 金:江苏省医学重点(实验室)学科-流行病学项目(ZDXKA2016008)~~
摘 要:目的廸立柱前衍生高效液相色谱法(high performance liquid chromatography,HPLC)测定保健食品中1-脱氧野尻霉素(1-deoxynojirimycin, 1-DNJ)的分析方法。方法样品经水超声提取20 min,在0.4 mol/L硼酸钾缓冲溶液(borate buffer solution,BBS)(pH=8.5)中,1-DNJ与5mmol/L芴甲氧羰酰氯(methoxycarbonyl chloride, FMOC-Cl)在20℃中水浴衍生30 min,滤液采用HPLC进行检测。以乙腈+磷酸水溶液为流动相,梯度洗脱。结果 1-DNJ在1.0~20.0μg/mL浓度范围内,线性关系良好,相关系数(r)=0.9993。回收率为90.96%~101.85%;相对标准偏差(relative standard deviation, RSD)为1.9%~3.4%。结论该方法前处理简便,结果准确,灵敏度较高,适用于保健食品中1-DNJ含量测定。Objective To establish a method for detection of 1-deoxynojirimycin (1-DNJ) in hypoglycemic health food by precolumn derivatization high performance liquid chromatography (HPLC). Methods The sample was ultrasonically extracted by water for 20 min. In 0.4 mol/L borate buffer solution (BBS) (pH=8.5), 1-DNJ and 5 mmol/L methoxycarbonyl chloride (FMOC-Cl) was heated in a water bath at 20 ℃ for 30 min and the filtrate was tested by HPLC. The gradient was eluted with acetonitrile+aqueous phosphoric acidas the mobile phase. Result 1-DNJ had good linearity in the concentration range of 1.0-20.0 μg/mL, and the correlation coefficient (r) was 0.9993. The recovery rate was 90.96%-101.85% and the relative standard deviation (RSD) was 1.9%-3.4%. Conclusion This method has the advantages of simple pretreatment, accurate result and high sensitivity, which is suitable for the determination of 1-DNJ content in health food.
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