UPLC-MS/MS法测定乳及乳制品中氯霉素残留前处理方法的比较  

Comparison of sample pretreatment methods in dairy products of chloramphenicol detemination by Ultra-High Performance Liquid Chromatography-electrospray ionization tandem mass spectrometry

作　　者：单艺[1] 亢美娟[1] 王象欣[1] 陈美君[1] 宋戈[1] 姜毓君[1] 

机构地区：[1]东北农业大学黑龙江省乳品工业技术开发中心,哈尔滨150028

出　　处：《中国乳品工业》2014年第3期54-58,共5页China Dairy Industry

基　　金：国家科技支撑计划(2012BAK17B04和2013BAD18B11)

摘　　要：通过比较3种不同的前处理方法，建立了超高压液相色谱一串联质谱法（UPLC-MS／MS）测定乳及乳制品中氯霉素的质量分数，以氯霉素一D5为同住素内标定量。测定氯霉素质量分数的方法。结果表明，对于液态乳制品，采用水：甲醇的溶液提取氯霉素．乙酸锌沉淀蛋白，HLB固相萃取柱富集净化。该方法前处理简单快速，对环境污染小，且检出限（以信噪比S／N=3计）为0．02μg／kg，添加回收率为86．7％90．7％，相对标准偏差（RSD）2．27％，适用于大量样品的集中测定。对于固态乳制品采用乙酸乙酯提取氯霉素．Silica固相萃取柱富集净化。该方法的检出限为0．1μg／kg，添加回收率为85．2％-90．2％，相对标准偏差（RsD）2．87％，稳定性高，适用于配方、工艺十分复杂的固态乳制品．A method of chloramphenicol determination in milk and dairy products using Ultra-High Performance Liquid chromatographyelectrospray ionization tandem mass spectrometry(UPLC-MS/MS) was developed by comparing three different extraction methods,which was quantitated with isotope internal standard of chloramphenicol-D5.It was indicated that,for liquid dairy products,water and methanol was used to extract chloramphenicol,zinc acetate was used to protein precipitation,HLB solid-phase extraction column was used for purification and enrichment. This pretreatment is simple and quick,small pollution to the environment,and the limit of detection(LOD,S/N=3) was 0.02 μg/kg,spiked recoveries was 86.7%~86.7%,relative standard deviation(RSD) was 2.27%,suitable for a large number of sample concentration determination. For solid-state dairy products,ethyl acetate was used to extract chloramphenicol,Silica column was used for purification and enrichment,the limit of detection(LOD,S/N =3) was 0.1 μg/kg,add recovery was 85.2% ~85.2%,relative standard deviation(RSD) was 2.87%. This method was high stability,suitable for the solid-state dairy products with complicated formulation and technology.

关 键 词：氯霉素 超高压液相色谱一串联质谱 同位素内标 乳制品 前处理 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]