摘要
本文建立了一种QuEChERS和C18固相萃取柱净化结合液相色谱串联质谱方法测定蚕砂中氯霉素残留。经乙酸乙酯提取,GCB和C18固相萃取柱净化,以甲醇和水为流动相梯度洗脱,C18柱(2.1 mm×100 mm,1.7μm)分离,在电喷雾离子源(ESI)负离子模式下采用液相色谱-串联质谱仪测定,内标法定量。结果显示,在0.02μg/L~5.00μg/L,氯霉素具有良好的线性关系,相关系数为1.000。氯霉素在4个加标水平(0.1μg/kg、0.3μg/kg、1.0μg/kg、2.0μg/kg)下回收率范围为74.7%~103.0%,RSD在4.36%~9.64%。该方法操作快速简单,且灵敏度与回收率高,可用于蚕砂中氯霉素残留的检测分析。
A method for the determination of chloramphenicol residues in silkworm excrement based on QuEChERS-High Performance liquid chromatography-tandem mass spectrometry was developed.The method was extracted by ethyl acetate,purified by GCB and C18 solid phase extraction column,eluted by methanol and water as mobile phase gradient,separated by C18 column(2.1 mm×100 mm,1.7μm),determined by liquid chromatography tandem mass spectrometry under the negative ion mode of electric spray ion source(ESI),and quantified by internal standard method.The results showed that chloramphenicol had a good linear relationship between 0.02μg/L-5.00μg/L with a correlation coefficient of 1.000.The recoveries of chloramphenicol at four supplemental levels(0.1μg/kg,0.3μg/kg,1.0μg/kg,2.0μg/kg)ranged from 74.7%-103.0%,and the RSD ranged from 4.36%-9.64%.The method is quick,simple,sensitive and has high recovery rate,so it can be used for the detection and analysis of chloramphenicol residues in silkworm excrement.
作者
梁香
崔凤云
朱绍华
付善良
成婧
陆静
焦艳娜
LIANG Xiang;CUI Fengyun;ZHU Shaohua;FU Shanliang;CHENG Jing;LU Jing;JIAO Yanna(Technology Center of Changsha Customs,Hunan Key Laboratory of Food Safety Science&Technology,Changsha Hunan,410004,China;Science and Technology Research Center of China Customs)
出处
《质量安全与检验检测》
2024年第2期1-7,共7页
QUALITY SAFETY INSPECTION AND TESTING
基金
海关总署科研项目(2023HK078)。
关键词
蚕砂
氯霉素
QUECHERS
固相萃取
液相色谱-串联质谱
Silkworm excrement
Chloramphenicol
QuEChERS
Solid phase extraction
High performance liquid chromatography-tandem mass spectrometry
