乳业科学与技术2025，Vol.48Issue(6)：30-35,6.DOI:10.7506/rykxyjs1671-5187-20250626-044
反相超高效液相色谱法测定乳粉中1-脱氧野尻霉素含量
Determination of 1-Deoxynojirimycin Content in Milk Powder by Reversed-Phase Ultra-high Performance Liquid Chromatography
摘要
Abstract
A reversed-phase ultra-high performance liquid chromatography method was established for the determination of 1-deoxynojirimycin(1-DNJ)in milk powder.The sample was extracted ultrasonically using a mixed solution of hydrochloric acid(0.01 mol/L)and methanol(1:1,V/V).After purification via low-temperature centrifugation,the extract was derivatized with 9-fluorenylmethoxycarbonyl chloride under alkaline conditions.Glycine was used to neutralize the derivatives,which was terminated by adding a 1%(V/V)acetic acid solution.The analyte was separated on a reversed-phase C18 column and detected using a diode array detector at a wavelength of 266 nm.Qualitative analysis was performed based on the retention time,and quantitative analysis was conducted using the external standard method.The results showed that the calibration curve exhibited a good linear relationship in the concentration range of 1-50 μg/mL.The limit of quantification was 18.0 mg/kg,and the limit of detection was 6.0 mg/kg.The recoveries of 1-DNJ from spiked samples at concentration levels of 18.0-270.0 mg/kg were 105.4%-106.6%,94.1%-97.4%,96.7%-102.7%,and 100.5%-104.5%with relative standard deviations of 1.18%,1.76%,2.08%,and 1.57%,respectively.This method is characterized by high sensitivity,accuracy and repeatability,and is suitable for the determination of the content of 1-DNJ in milk powder.关键词
乳粉/1-脱氧野尻霉素/反相超高效液相色谱/衍生/二极管阵列检测器Key words
milk powder/1-deoxynojirimycin/reversed-phase ultra-high performance liquid chromatography/derivatization/diode array detector分类
轻工纺织引用本文复制引用
陈静,段国霞,刘丽君,吴晓莉,吕志勇,胡雪..反相超高效液相色谱法测定乳粉中1-脱氧野尻霉素含量[J].乳业科学与技术,2025,48(6):30-35,6.基金项目
内蒙古自治区重点研发和成果转化计划项目(2023YFHH0093) （2023YFHH0093）
