食品中焦糖色与4-甲基咪唑的测定  

Determination of Caramel Color and 4-Methylimidazole Content in Food

作　　者：叶佳明 钟世欢 苏敏 秦芸桦 黄南 杨天明 巩启强 王森燚 YE Jiaming;ZHONG Shihuan;SU Min;QIN Yunhua;HUANG Nan;YANG Tianming;GONG Qiqiang;WANG Senyi(Zhejiang Gongzheng Testing Center,Co.,Ltd.,Hangzhou 310009,China;Zanyu Technology Group Co.,Ltd.,Hangzhou 310009,China)

机构地区：[1]浙江公正检验中心有限公司,浙江杭州310009 [2]赞宇科技集团股份有限公司,浙江杭州310009

出　　处：《食品科技》2024年第5期321-327,共7页Food Science and Technology

基　　金：赞宇科研基金项目(2023005)。

摘　　要：文章建立了高效液相色谱法测定食品中焦糖色的含量,结合超高效液相色谱-串联质谱法测定其4-甲基咪唑的含量的方法。样品加入水超声提取后,离心,上清液经MCX柱纯化后,收集初始流出液以4倍乙醇沉淀,离心后弃去上清液,沉淀以水复溶后测定焦糖色素;4-甲基咪唑收集氨水甲醇洗脱液,氮吹后以初始流动相复溶。焦糖色素以10 mmol/L磷酸二氢钠溶液为流动相,采用资生堂SCX色谱柱(4.6 mm×150 mm,5 μm),等度洗脱,610 nm波长下测定。4-甲基咪唑以含0.1%甲酸10 mmol/L乙酸铵水溶液和乙腈为流动相梯度洗脱,经资生堂HILIC色谱柱(2.1 mm×100 mm,3 μm)色谱柱分离后,采用多反应监测模式进行定量分析,内标法定量。焦糖色素与4-甲基咪唑在各自浓度范围线性良好,三水平加标回收结果显示,焦糖色素的平均回收率为80.5%~94.2%,相对标准偏差为3.3%~7.8%,固体类样品检出限为0.02 g/kg,液体类样品检出限为0.02 g/L。4-甲基咪唑的平均回收率为85.3%~106.2%,相对标准偏差为3.1%~6.9%,固体类样品检出限为1.0 μg/kg,液体类样品检出限1.0 μg/L。该方法优化前处理过程与仪器色谱条件,较好地控制了基质干扰,具有灵敏度高、重现性好、抗干扰能力强等特点,适用于酱油、米醋、可乐和黄酒等食品中焦糖色与4-甲基咪唑的检测。A high performance liquid chromatography (HPLC) method for determining the content of caramel color in food was established,combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for determining the content of 4-methylimidazole.After adding water for ultrasonic extraction,the sample was centrifuged and the supernatant was purified by MCX column.The initial effluent was collected and precipitated with 4 times ethanol.After centrifugation,the supernatant was discarded and the precipitate was redissolved in water before measuring caramel color,4-methylimidazole collects ammonia water methanol eluate,and after nitrogen blowing,it was redissolved in the initial mobile phase.Caramel color was prepared using a 10 mmol/L sodium dihydrogen phosphate solution as the mobile phase using a Shiseido SCX column (4.6 mm×150 mm,5 μm).Using a chromatographic column with equal elution,measure at a wavelength of 610 nm.4-methylimidazole was eluted with a gradient of 10 mmol/L ammonium acetate aqueous solution containing 0.1% formic acid and acetonitrile as the mobile phase,and passed through a Shiseido HILIC column (2.1 mm×100 mm,3 μm).After chromatographic column separation,quantitative analysis was performed using a multi reaction monitoring mode and internal standard method.Caramel color and 4-methylimidazole showed good linearity in their respective concentration ranges.The results from three-level spiked recoveries showed that the average recovery rates from caramel color were 80.5%–94.2%,with relative standard deviations of 3.3%–7.8%.The detection limit for solid samples were 0.02 g/kg,and for liquid samples were 0.02 g/L.The average recovery rates of 4-methylimidazole were 85.3%–106.2%,with a relative standard deviations of 3.1%–6.9%.The detection limit for solid samples were 1.0 μg/kg,detection limit for liquid samples were 1.0 μg/L.This method optimizes the pre-treatment process and instrument chromatographic conditions,effectively controls matrix interference,a

关 键 词：焦糖色 4-甲基咪唑 高效液相色谱 液质联用 

分 类 号：TS207.3[轻工技术与工程—食品科学]