基于QuEChERS测定鸡肉中22种磺胺类药物残留  

Determination of 22 sulfonamides residues in chicken based on QuEChERS

作　　者：吴香伦 周华[1] 姚熙霖 黄琴 刘倩 周佳莉 WU Xiang-lun;ZHOU Hua;YAO Xi-lin;HUANG Qin;LIU Qian;ZHOU Jia-li(Quzhou Municipal Center for Disease Control and Prevention,Zhejiang 324000,China;不详)

机构地区：[1]衢州市疾病预防控制中心,浙江324000 [2]常山县疾病预防控制中心

出　　处：《中国卫生检验杂志》2023年第14期1686-1692,共7页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立基于QuEChERS结合液相色谱-串联质谱快速测定鸡肉中22种磺胺类药物残留的方法。方法通过对流动相的种类、提取溶剂的种类、盐析剂、吸附剂的种类和用量、定容液的种类进行讨论,在加标量为10μg/kg的条件下,改变各优化条件,以回收率为指标得出最优的前处理条件。并分析该方法的基质效应、线性关系、检出限、定量限、加标回收率和相对标准偏差(RSD),以评价方法的可行性。最后将该方法用于实际样品的检测。方法以甲醇和0.1%甲酸水溶液为流动相,样品经1%甲酸乙腈提取,2 g氯化钠(NaCl)为盐析剂,20 mg C18,10 mg PSA为净化剂,经LC-MS/MS检测,用基质匹配曲线内标法定量。结果22种磺胺类药物在0.1μg/L~20μg/L内的线性相关系数均大于0.9988,方法检出限与定量限分别为0.11μg/kg~1.66μg/kg和0.35μg/kg~2.23μg/kg。在2μg/kg、10μg/kg、50μg/kg 3个加标水平上,平均回收率为75.6%~124.0%,RSD为1.1%~15.7%。结论本方法快速简便、准确可靠,可用于鸡肉中的22种磺胺类药物残留的快速分析。Objective This paper aims to establish a rapid method for the determination of 22 sulfonamides residues in chicken based on QuEChERS method combined with liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods The types of mobile phase,extraction solvent,salting out agent,sorbent and constant volume liquid were discussed.Under the condition of adding 10μg/kg,the optimization conditions were changed,and the optimal pre-treatment conditions were obtained with the recovery rate as the index.The matrix effect,linear relationship,detection limit,quantitative limit,recovery rate and relative standard deviation(RSD)of the method were analyzed to evaluate the feasibility of the method.Finally,the method is applied to the detection of real samples.Methanol and 0.1% formic acid aqueous solution were used as mobile phase,the samples were extracted by 1%acetonitrile,2 g sodium chloride(NaCl)as salting agent,20 mg C18,10 mg PSA as purification agent,detected by LC-MS/MS,and quantified by matrix matching curve internal standard method.Results The linear correlation coefficients(r)of 22 sulfonamides in the range of 0.1μg/L to 20.0μg/L were all greater than 0.9988,and the limits of detection and quantitation were within 0.11μg/kg-1.66μg/kg and 0.35μg/kg-2.23μg/kg,respectively.The average recoveries were 75.6%-124.0% and RSDs were 1.1%-15.7% at the spiked levels of 2μg/kg,10μg/kg and 50μg/kg.Conclusion The method is simple,accurate and reliable,and can be used for the rapid detection of 22 sulfonamides residues in chicken.

关 键 词：QUECHERS 液相色谱-质谱联用 鸡肉 磺胺 

分 类 号：O657[理学—分析化学]