摘要
通过“dip-coating”法制备了一种表面覆盖聚丙烯腈(PAN)/亲水-疏水平衡颗粒(HLB)涂层的棉签固相微萃取(SPME)。该棉签SPME制作方法简便、成本低廉(1元/支)、可重复使用,并可实现样品前处理的半自动化。通过优化PAN和HLB的组成比例,使棉签SPME对9种大环内酯类抗生素标准品的吸附率达到80%以上,解吸率达到99%以上。使用棉签SPME结合高效液相色谱-串联质谱法(HPLC-MS/MS),同时检测蜂蜜中9种大环内酯类抗生素(MACs)。9种MACs在1~20μg/L浓度范围内呈良好线性关系,线性相关系数(R2)均大于0.9978。9种MACs在1, 5, 10μg/kg 3个标准添加浓度下的平均回收率为71.8%~86.4%,相对标准偏差(RSD)为2.2%~5.3%,检出限(LOD)为0.24~1.35μg/kg,定量限(LOQ)为1.02~4.62μg/kg。
A cotton swab based solid-phase microextraction(SPME)covered with polyacrylonitrile(PAN)/hydrophilic-hydrophobic balance(HLB)particles,which is simple,inexpensive,broadly applicable,reusable,and semi-automated for sample pretreatment,was prepared by the dip-coating method.By optimizing the composition ratio of PAN and HLB,the adsorption rate of swab SPME for nine macrolide antibiotic standards reached more than 80%and the desorption rate more than 99%.Detection of 9 macrolide antibiotics(MACs)in honey was performed using this SPME in combination with HPLC-MS/MS.The nine MACs showed good linearity in the concentration range of 1-20μg/L,with linear correlation coefficients(R 2)greater than 0.9978.The average recoveries of the nine MACs at the three spiked standard concentrations of 1,5,10μg/kg ranged from 71.8%to 86.4%,with the relative standard deviations(RSDs)of 2.2%-5.3%.The limits of detection(LODs)were 0.24-1.35μg/kg and the limits of quantification(LOQs)were 1.02-4.62μg/kg.
作者
宫小明
李凯
许文娟
王洪涛
刘孟孝
孔彩霞
GONG Xiaoming;LI Kai;XU Wenjuan;WANG Hongtao;LIU Mengxiao;KONG Caixia(Comprehensive Technical Service Center of Weifang Customs,Weifang 261041,China)
出处
《分析试验室》
EI
CAS
CSCD
北大核心
2024年第4期535-540,共6页
Chinese Journal of Analysis Laboratory
基金
海关总署科研项目(2020HK201,2022HK030)资助。
关键词
大环内酯类抗生素
固相微萃取
蜂蜜
高效液相色谱-串联质谱
macrolide antibiotics
solid-phase microextraction
honey
high performance liquid chromatographytandem mass spectrometry(HPLC-MS/MS)
