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.
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)
出处
《中国乳品工业》
CAS
北大核心
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)。
