液相色谱-串联质谱同时测定家禽组织中16种磺胺残留  

Simultaneous Determination of 16 Sulfonamides in Poultry Meat by High-Performance Liquid Chromatography- Tandem Mass Spectrometry

作　　者：庞国芳[1] 曹彦忠[1] 张进杰[1] 贾光群[1] 范春林[1] 李学民[1] 刘永明[1] 石玉秋[1] 

机构地区：[1]秦皇岛出入境检验检疫局,秦皇岛066002

出　　处：《分析化学》2005年第9期1252-1256,共5页Chinese Journal of Analytical Chemistry

摘　　要：5 g 家禽组织样品,用乙腈提取,旋转蒸发器减压蒸干后,用乙腈-0.01 mol/L 乙酸铵溶液溶解(12:88,V/V),用正己烷去除脂肪后,样液用高效液相色谱分离,电喷雾串联四级杆质谱进行检测,外标法定量.本方法研究的16种磺胺(磺胺甲噻二唑、磺胺醋酰、磺胺嘧啶、磺胺氯哒嗪、磺胺甲基异噁唑、磺胺甲基嘧啶、磺胺吡啶、磺胺二甲异噁唑、磺胺-6-甲氧嘧啶、磺胺邻二甲氧嘧啶、磺胺甲氧哒嗪、磺胺间二甲氧嘧啶、磺胺噻唑、磺胺二甲嘧啶、磺胺甲氧嘧啶、磺胺苯吡唑)的线性范围为0.2～120 ng,线性相关系数r>0.995;在2.5～600 μg/kg的4个添加水平范围内的平均回收率为75.4%～97.3%;相对标准偏差为3.48%～14.09%;方法检出限(LOD)为1.0～12.0 μg/kg;方法定量限(LOQ)为2.0～24.0 μg/kg.Five gram poultry meat samples were weighed and extracted with acetonitrile. Then the sample solution was evaporated to dryness on the rotary evaporator and the residues dissolve in acetonitrile ＋ 0.02 mol/L acetic ammonium solutions （12：88） was remove at in sample solution by hexane. High performance liquid chromatographic Cls column was applied for separation before submitting for determination by elelctronsprayionization-mas spectrometry-mass spectrometry. The linear ranges of the sulfamethizole, sulfacetamide, sulfapyridine, sulfadiazine, sulfachloropyridazine, sulfamethoxazole, sulfamerazine, sulfisoxazole, sulfamonomethoxine , sulfadoxine, sulfamethoxypyridazine, sulfadimethoxine, sulfathiazole, sulfamethazine, sulfameter and sulfaphenazole are between 0.2 and 120 ng, and the linear correlation coefficient r 〉0. 995. In the ranges of 2.5 - 600μg/kg, mean fortification recoveries are between 75.4% and 97.3% , the relative standard deviation are 3.5% - 14. 1%. Limits of detection and quantitation for the method are 1.0 - 12.0μg/kg, 2.0 - 24.0μg/kg, respectively.

关 键 词：液相色谱-串联质谱 家禽组织 16种磺胺 液相色谱分离 磺胺嘧啶 串联质谱 同时测定 组织 家禽 磺胺甲基嘧啶 

分 类 号：O657.63[理学—分析化学] TQ577.13[理学—化学]