高效液相色谱串联质谱法测定牛奶中四环素类抗生素及其代谢产物  

Determination of Multi-Residues of Tetracyclines and Their Metabolites in Milk by High Performance Liquid Chromatography-Tandem Positive-ion Electrospray Ionization Mass Spectrometry

作　　者：岳振峰[1] 邱月明[2] 林秀云[1] 吉彩霓[1] 

机构地区：[1]深圳出入境检验检疫局食品检验检疫技术中心,深圳518067 [2]中国检验检疫科学研究院检测新技术与装备研究所,北京100025

出　　处：《分析化学》2006年第9期1255-1259,共5页Chinese Journal of Analytical Chemistry

基　　金：科技部"十五"食品安全重大专项课题资助项目(No.2001BA804A18-12)

摘　　要：建立了牛奶中四环素、金霉素、土霉素、强力霉素、去甲基金霉素、甲烯土霉素和二甲胺四环素等7种四环素类抗生素及差向四环素、差向金霉素、差向土霉素等3种代谢产物多残留的液相色谱串联质谱同时测定方法。方法采用Inertsil C8—3（5μm，150mm×2．1mmi．d）反相色谱柱，以pH4．0的EDTA—Mcllvaine缓冲溶液为提取溶液，以HLB固相萃取柱为净化柱，流动相为甲醇＋0．01mol／L三氟乙酸（梯度洗脱），流速0．3mL／min，以正离子多反应监测模式测定，进样量30μL。方法的检出限为0．5～10μg／kg；测出限为50μg／kg；线性范围为50～1200μg／L，加标回收率为74．4％～101％，相对标准偏差为1．8％～8．3％。本方法具有灵敏、准确、简便、快速等优点，适用于牛奶中四环素类抗生素及其代谢产物多残留的同时确证检测。A high performance liquid chromatography-tandem mass spectrometric （HPLC/MS/MS） method was developed for the simultaneous determination of 7 antibiotics residues of tetracycline, chlortetracycline, oxytetracycline, doxycycline, demeclocycline, methacycline, minocycline and 3 metabolites of 4-epitetracycline, 4-epichlortetracycline, 4-epioxytetracycline in milk. In the method, the reversed-phase column of Inertsil C8-3 （5 μm, 150 mm ×2.1 mm i. d）, the EDTA-Mcllvaine buffer extraction solution （pH 4.0）, the HLB solid phase extraction column, the methanol-0.01 mol/L trifluoroacetic acid solution mobile phase with gradient elution were used. The flow rate was 0.3 mL/min, the detection mode was multiple reaction monitoring with positive-ion electrospray ionization, and the injection volume is 30 μL. The limit of detection （LOD） is between 0.5 and 10.0 μg/kg, and the limit of quantitation （LOQ） is 50 μg/kg. The linear plots are obtained between 50 and 1200 μg/kg. Overall recoveries are between 74.4% and 101% with a RSD （n = 10） of 18% -8.3%. The method is sensitive, accurate, convenient and fast, and can be used to simultaneously confirm multi-residue of tetracyclines and their metabolites in milk.

关 键 词：高效液相色谱串联质谱 四环素类 代谢产物 残留 牛奶 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]