高效液相色谱-质谱法测定生鲜乳中氯霉素的方法研究  

Study on the method for determining chloramphenicol in fresh milk by high performance liquid chromatography mass spectrometry

作　　者：黄鑫 廖欢 陈灵 栾庆祥 周泽晓 章厉劼 杨强 金晓峰 HUANG Xin;LIAO Huan;CHEN Ling;LUAN Qinxiang;ZHOU Zexiao;ZHANG Lijie;YANG Qiang;JIN Xiaofeng(Guizhou Instiute for Veterinary Drug Feed Festing,Guiyang 550003,China)

机构地区：[1]贵州省兽药饲料检测所,贵阳550003

出　　处：《中国乳品工业》2024年第4期61-64,共4页China Dairy Industry

基　　金：贵州省农业农村厅科技项目(黔农牧[2021]002号)。

摘　　要：建立高效液相色谱-串联质谱法测定生鲜乳中氯霉素残留的方法。对GB 29688—2013《牛奶中氯霉素残留量的测定液相色谱-串联质谱法》中的测定方法进行优化。量取生鲜乳适量,加氯霉素-D_(5)内标工作液,经乙腈萃取后,5000 r/min离心,过OASIS Prime HLB柱,将所过溶液氮气吹干,水复溶,取下层水溶液层过0.22μm水系滤膜。将C_(18)柱作为液相色谱柱,按V_((乙腈))∶V_((水))=60:40体积比等度洗脱。结果表明,氯霉素在0.2~10.0μg/kg范围内有较好的准确度,相关系数均大于0.99,方法检测限0.05μg/kg,定量限都为0.2μg/kg,3个加标浓度(0.2、1.0、10.0μg/kg)的氯霉素的平均回收率为85.5%~116.0%,相对标准偏差为1.23%~8.16%。试验结果完全符合国家标准检测要求,适用于生鲜乳中氯霉素定性定量快速检测。To establish a method for the determination of chloramphenicol residues in fresh milk by UPLC MS/MS.The determination method in Determination of Chloramphenicol Residue in Milk by UPLC MS/MS(GB 29688-2013)was optimized.Take an appropriate amount of fresh milk,add chloramphenicol-D_(5) internal standard,extract it with acetonitrile,centrifugate it at 5000 r/min,pass it through OASIS Prime HLB column,blow the solution dry with nitrogen,redissolve it in water,take the lower layer of aqueous solution and pass it through 0.22μm aqueous filter membrane.Take C_(18) column as the liquid chromatographic column,elute according to the volume ratio of acetonitrile:water(60:40).The accuracy of chloramphenicol was better in the range of 0.2-10.0μg/kg,and the correlation coefficients were greater than 0.99.The detection limit was 0.05μg/kg,and the quantification limit was 0.2μg/kg.The average recovery of chloramphenicol at three spiked concentrations(0.2,1.0,10.0μg/kg)was 85.5%-116.0%,and the relative standard deviation was 1.23%-8.16%.The test results fully meet the requirements of relevant national standards for the detection of fresh milk,and are suitable for the qualitative and quantitative detection of chloramphenicol in fresh milk.

关 键 词：高效液相色谱-质谱法 测定 生鲜乳 氯霉素 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]