摘要
建立了猪肉中磺胺类兽药残留基体标准物质高准确度定值方法,优化了提取溶剂、提取次数、添加内标试剂后的平衡时间和过滤膜的选择等样品前处理条件。猪肉样品中加入同位素标记物,乙腈提取3次,上清液过无水硫酸钠柱,提取物经50℃水浴旋转蒸发至干,正己烷饱和的流动相定容溶解,正己烷脱脂净化,然后正离子多反应监测测定,最后采用外标法定量。结果表明,磺胺嘧啶和磺胺二甲嘧啶在10. 0～200. 0 ng/m L浓度范围内呈良好的线性关系,线性相关系数均大于0. 999,方法的检出限和定量限分别为0. 5、2. 0μg/kg,在低、中、高3个添加水平范围内的回收率为95. 7%～104. 8%,相对标准偏差<5%(n=6),可用于猪肉中磺胺类兽药残留基体标准物质均匀性检验、稳定性监测和定值。
A highly accurate quantification method was established for the determination of sulfonamides residues in pork for a matrix reference material. Several key issues during the sample pretreatment were optimized including extraction solvent,times of sample extraction,equilibration time after the addition of internal standards,the selection of filter membrane. Internal standards were added into the sample,and then the sample was extracted 3 times by acetonitrile and centrifugation.The supernatant was then treated with a home-made separation column filled with anhydrous sodium sulfate.The extract was evaporated and dried by rotary evaporator at the temperature of 50 ℃.The residue was dissolved by mobile phase saturated with n-hexane,and it was defatted and purified by n-hexane.The analysis was performed under the positive mode using multiple reaction monitoring(MRM) and quantified by external standard method.A good linearity was obtained in the range from 10. 0 to 200. 0 ng/m L for sulfadiazine and sulfadimidine,while the correlation coefficients were more than 0. 999.The limits of detection(LODs) and the limits of quantitation(LOQs) were 0. 5 μg/kg and 2. 0 μg/kg respectively. The recovery rates at the three spiked levels were between 95. 7% ~104. 8% with relative standard deviations(RSDs,n = 6) less than 5%.The method was suitable for the homogeneity inspection,stability monitoring and certify value of the matrix reference materials for sulfonamides residues in pork.
作者
段嫚雷
李兰英
李杰
闻艳丽
孟娇然
王乐乐
丁敏
刘刚
DUAN Man-lei;LI Lan-ying;LI Jie;WEN Yan-li;MENG Jiao-ran;WANG Le-le;DING Min;LIU Gang(Shanghai Institute of Measurement and Testing Technology,Shanghai 201203,China)
出处
《化学试剂》
CAS
北大核心
2019年第3期263-269,共7页
Chemical Reagents
基金
上海市质量技术监督局科研项目(2016-06)
关键词
磺胺
兽药残留
基体标准物质
高准确度
sulfonamides
residues
matrix reference material
high accuracy
