气相色谱-质谱法测定食品接触材料及制品中4种柠檬酸酯类化合物的迁移量  

Determination of migration of four citrate compounds in food contact mal als and products by gas chromatography-mass spectrometry method

作　　者：刘仕途 曾铭 陈湘颖 李丹 董犇 阿文伟 钟怀宁 IU Shitu;ZENG Ming;CHEN Xiangying;LI Dan;DONG Ben;A Wenwei;ZHONG Huaining(Guangzhu Customs Technical Center,Guangzhou 510070,China)

机构地区：[1]广州海关技术中心,广州510070

出　　处：《分析试验室》2024年第4期463-468,共6页Chinese Journal of Analysis Laboratory

基　　金：国家重点研发项目(2022YFF0607202)资助。

摘　　要：建立了测定食品接触材料及制品中柠檬酸三乙酯(TEC)、乙酰柠檬酸三乙酯(ATEC)、柠檬酸三丁酯(TBC)和乙酰柠檬酸三丁酯(ATBC)迁移量的气相色谱-质谱(GC-MS)法。食品接触材料样品经迁移试验后,所得水基浸泡液和橄榄油浸泡液分别经正己烷和乙腈萃取后测定,95%乙醇浸泡液和异辛烷浸泡液直接测定。结果表明,4种目标化合物的标准工作曲线在0.2~2.0 mg/L浓度范围内线性关系良好,相关系数(r^(2))大于0.995;4种柠檬酸酯类化合物在4%乙酸、 10%乙醇、 20%乙醇、 50%乙醇、 95%乙醇、异辛烷、橄榄油等模拟物中的检出限为0.05~0.11 mg/L,定量限为0.15~0.30 mg/L。对基质空白浸泡液进行低、中、高3个浓度水平添加实验,加标回收率在90.6%~110%之间,相对标准偏差(RSD)为0.9%~8.6%。该方法能够满足食品接触材料及制品中4种柠檬酸酯类化合物迁移量检测的需求。A gas chromatography-mass spectrometry(C-MS)method was established to determine the migration of triethyl citrate(TEC),acetyl triethyl citrate(ATEC),tributyl citrate(TBC),and acetyl tributyl citrate(ATBC)in food contact materials and products.After the migration test of food contact material samples,the obtained water-based soaking solution and the olive oil soaking solution were extracted with n-hexane and acetonitrile respectively,and then determined by GC-MS,while the 95%ethanol soaking solution and isooctane soaking solution were directly determined by GC-MS.The results showed that the method had correlation coefficients(P)greater than 0.995.The detection limits of four citrate compounds in 4%acetic acid,10%ethanol,20%ethanol,50%ethanol,95%ethanol,isooctane,and olive oil simulants were 0.05-0.11 mg/L,the limits of quantification were 0.15-0.30 mg/L,and the linear ranges were 0.2-2.0 mg/L.The average spiked recoveries of this method at low,medium,and high levels were 90.6%-110%,and the relative standard deviations(RSDs)were 0.9%-8.6%.This method can meet the requirements for determination of the migration amounts of four citrate compounds in food contact materials and their products.

关 键 词：柠檬酸三乙酯(TEC) 乙酰柠檬酸三乙酯(ATEC) 柠檬酸三丁酯(TBC) 乙酰柠檬酸三丁酯(ATBC) 食品接触材料 气相色谱-质谱法(GC-MS) 

分 类 号：O657.71[理学—分析化学] O622.3[理学—化学]