色谱2024，Vol.42Issue(8)：792-798,7.DOI:10.3724/SP.J.1123.2023.10016
柱前衍生-高效液相色谱-荧光检测法测定白酒中的甜蜜素
Determination of sodium cyclamate in Baijiu by pre-column derivatization-high performance liquid chromatography with fluorometric detection
摘要
Abstract
Sodium cyclamate in Baijiu is a key item in the China National Food Safety Supervi-sion and Inspection Plan.A simple,economical,sensitive,and reliable method is urgently nee-ded for routine analysis and internal quality control.A method based on high performance liquid chromatography with fluorescence detection(HPLC-FLD)was developed for the determination of sodium cyclamate in Baijiu by o-phthalaldehyde derivatization.First,the sodium cyclamate in the sample solution was converted into amino compounds using the desulfurization reaction under acidic conditions.Next,400 g/L sodium hydroxide solution was added to the sample so-lution for neutralization.The amino compounds in the sample solution were then derivatized with o-phthalaldehyde to produce indole-substituted derivatives that are capable of producing fluorescence signals.Separation was carried out on a C18 column(250 mm×4.6 mm,5 μm)in isocratic elution mode using a mobile phase consisting of acetonitrile and phosphate buffer.Fi-nally,the eluate was monitored using a fluorescence detector,and an external standard method was used for quantification.A good linear relationship was obtained in the range of 0.1-2.0 mg/L,with correlation coefficients greater than 0.999.The average recoveries of sodium cycla-mate spiked at levels of 0.1-1.0 mg/kg in Baijiu samples ranged from 90.7％to 100.9％,with relative standard deviations(RSDs)of 3.5％-5.6％(n=6).The limits of detection and quanti-fication were 0.03 and 0.10 mg/kg,respectively.Nine Baijiu samples collected from the market were tested,and the results demonstrated that the contents of sodium cyclamate detected by the developed method were consistent with those obtained using the liquid chromatography-tandem mass spectrometry(LC-MS/MS)method described in GB 5009.97-2016(the third method).The proposed method is economical,sensitive,specific,and accurate;thus,it pro-vides a basic approach for the determination of sodium cyclamate in Baijiu samples and has great potential for routine analysis in foodstuffs.关键词
高效液相色谱/荧光检测/柱前衍生/甜蜜素/白酒Key words
high performance liquid chromatography(HPLC)/fluorescence detection/pre-column derivatization/sodium cyclamate/Baijiu分类
化学化工引用本文复制引用
顾长瑜,李晓斌,柴晓,王真,侯晨宇,柯润辉..柱前衍生-高效液相色谱-荧光检测法测定白酒中的甜蜜素[J].色谱,2024,42(8):792-798,7.基金项目
国家重点研发计划项目(2020YFE0203500).National Key Research and Development Program of China(No.2020YFE0203500). （2020YFE0203500）
