液相色谱―串联质谱法测定鸡肉中22种磺胺及其增效剂残留量.docVIP

液相色谱―串联质谱法测定鸡肉中22种磺胺及其增效剂残留量 　　摘 要：建立鸡肉中22种磺胺及其增效剂多残留检测的液相色谱-串联质谱法。样品经过甲酸-乙腈（1∶199，V/V）溶液提取，正己烷脱脂，液-液分配净化后，C18柱分离，甲醇、水-甲酸水溶液（体积分数0.1%）为流动相梯度洗脱，采用电喷雾电离源（electrospray ionization，ESI）正离子多反应检测（multiple reaction monitoring，MRM）模式检测，外标法定量。结果表明：药物在2.0～100.0 μg/L质量浓度范围内线性关系良好，相关系数均大于0.99，方法的检出限和定量限分别为0.5 μg/kg和2.0 μg/kg，在添加量为2.0、5.0、10.0 μg/kg时回收率为61.8%～88.3%，相对标准偏差小于11.3%。该方法简便快捷，可用于鸡肉中磺胺类药物及其增效剂的多残留检测。 中国论文网 /8/view-7177553.htm 　　关键词：液相色谱-串联质谱；鸡肉；磺胺；增效剂 　　Determination of Residues of 22 Sulfonamides and One Sulfonamide Potentiator in Chickens by Liquid Chromatography-Tandem Mass Spectrometry 　　WEI Yunji1，ZHU Zhenyi1，FENG Min1，ZHANG Ke1， WANG Xiaojin1，HE Jian1，WEI Bin1，DING Tao2 　　（1.Huaian Entry-Exit Inspection and Quarantine Bureau，Huaian223001，China；2.Animal，Plant and Food Inspection Center（APFIC）， Jiangsu Entry-Exit Inspection and Quarantine Bureau，Nanjing 210001，China） 　　Abstract： A multi-residue analytical method for the determination of 22 sulfonamides and 1 sulfonamide potentiator in chicken was developed by liquid chromatography-tandem mass spectrometry （LC-MS）. The sample was extracted with formic acid-acetonitrile （1：199， V/V）， and the extract was defatted with n-hexane and cleaned up by liquid-liquid partition. The analytes were separated on a C18 column using a mobile phase consisting of methanol and water containing 0.1% （V/V） formic acid with gradient elution. The anaysis of the 23 analytes was performed by electrospray ionization （ESI） mass spectrometry under the positive mode using multiple reaction monitoring （MRM） and quantified by external standard method. The calibration curves showed good linearity. The limit of detection （LOD） and limit of quantitation （LOQ） were 0.5 and 2.0 μg/kg， respectively. At the spiked levels of 2.0， 5.0 and 10.0 μg/kg， recoveries ranged from 61.8% to 88.3%， with relative standard deviations （RSD） less than 11.3%. This method is convenient and suitable for the determination of residues of sulfonamides and the potentiator