高效液相色谱法测定食品接触用涂料中2-甲基咪唑、4-甲基咪唑和1-乙烯基咪唑的含量  

Determination of 2-Methylimidazole,4-Methylimidazole and 1-Vinylimidazole in Food Contact Coatings by High Performance Liquid Chromatography

作　　者：王乐 项海波 张丽 WANG Le;XIANG Haibo;ZHANG Li(Technical Center of Jinan Customs,Jinan 250014,China;Technical Center of Qingdao Customs,Qingdao 266599,China)

机构地区：[1]济南海关技术中心,济南250014 [2]青岛海关技术中心,青岛266599

出　　处：《理化检验(化学分册)》2025年第2期213-218,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：海关总署科研项目(2020HK247);济南海关科研项目(2020JK010)。

摘　　要：取0.500 g溶剂型食品接触用涂料样品,加入5 mL乙酸乙酯,超声提取15 min,加入20 mL甲醇,离心10 min。取0.500 g水性食品接触用涂料样品,加入25 mL甲醇,涡旋1 min,超声提取15 min,离心10 min。所得上清液均过0.22μm有机滤膜,滤液采用高效液相色谱仪分析。以Acclaim^(TM) 120 C_(18)色谱柱为固定相,以体积比1∶9的乙腈-0.05%(体积分数)氨水溶液的混合溶液为流动相,在1.0 mL·min^(-1)流量下等度洗脱分离3种咪唑类化合物,在检测波长211 nm(2-甲基咪唑、4-甲基咪唑)和227 nm(1-乙烯基咪唑)下测定。结果显示,3种咪唑类化合物的质量浓度均在一定范围内和峰面积呈线性关系,测定下限(10S/N)为5.0~20.0 mg·kg^(-1)。按照标准加入法进行回收试验,回收率为92.5%~108%,测定值的相对标准偏差(n=6)均不大于2.5%。An aliquot(0.500 g)of solvent-based food contact coating sample was taken,and 5 mL of ethyl acetate was added.After ultrasound for 15 min,20 mL of methanol was added,and the mixture was centrifuged for 10 min.An aliquot(0.500 g)of water-based food contact coating sample was taken,and 25 mL of methanol was added.The mixture was vortexed for 1 min,extracted by ultrasound for 15 min,and centrifuged for 10 min.The supernatant obtained was passed through an 0.22μm organic filter membrane,and the filtrate was analyzed by high performance liquid chromatography.Using Acclaim^(TM) 120 C_(18) chromatographic column as stationary phase,and the mixed solution composed of acetonitrile and 0.05%(volume fraction)aqueous ammonia solution at a volume ratio of 1∶9 as mobile phase,3 imidazole compounds were separated by isocratic elution at a flow rate of 1.0 mL·min^(-1).Determination was made at detection wavelengths of 211 nm(2-methylimidazole and 4-methylimidazole)and 227 nm(1-vinylimidazole).It was shown that linear relationships between values of the mass concentrations and peak areas of 3 imidazole compounds were kept in definite ranges,with lower limits of determination(10S/N)in the range of 5.0-20.0 mg·kg^(-1).Test for recovery was made according to the standard addition method,giving recoveries in the range of 92.5%-108%,and RSDs(n=6)of the determined values were not more than 2.5%.

关 键 词：高效液相色谱法 溶剂型食品接触用涂料 水性食品接触用涂料 2-甲基咪唑 4-甲基咪唑 1-乙烯基咪唑 

分 类 号：O657.7[理学—分析化学]