摘要
为了实现蜂蜜中多种抗生素的残留量同时测定,优化前处理流程,合成了一种新型的多孔聚合物材料(POP),应用于检测蜂蜜中的11种抗生素残留。前处理采用多孔聚合物材料分散吸附方式,液相色谱串联质谱以0.1%(v/v)甲酸水溶液和乙腈为流动相进行洗脱,AtiantisR T3色谱柱(2.1 mm×50 mm,1.7μm)分离,11种抗生素可在4 min内达到良好分离效果。四环素类、磺胺类、喹诺酮类药物分别在10~500、2~100和1~50μg/L范围内线性关系良好,检出限分别为3.0、0.6和0.3μg/kg,定量限分别为10.0、2.0和1.0μg/kg。11种抗生素在低、中、高三水平加标下的平均回收率为90.9%~108.7%,相对标准偏差为2.1%~9.4%。相较于传统固相萃取净化方式,使用POP的检测方法具有操作便捷、节能高效的特点;且重复性好,回收率高,可用于蜂蜜中多种抗生素残留的检测。
In order to achieve simultaneous determination of various antibiotic residues in honey and optimize the pre-treatment process,a novel porous organic polymer material(POP)was synthesized and applied to detect 11 antibiotic residues in honey.The pre-treatment was carried out using a porous polymer material dispersion adsorption method.Liquid chromatography tandem mass spectrometry was performed with a 0.1%(v/v)formic acid aqueous solution and acetonitrile as the mobile phase for elution.The AtiantisR T3 column(2.1 mm x 50 mm,1.7μm)was used for separation of antibiotics residues,and the 11 antibiotics achieved good separation results within 4 minutes.Tetracyclines,sulfonamides,and quinolones had good linear relationships within the range of 10 to 500,2 to 100,and 1 to 50μg/L,respectively.Their limits of detection were 3.0,0.6,and 0.3μg/kg,respectively.Their limits of quantification reached 10.0,2.0,and 1.0μg/kg,respectively.The average recovery rates of 11 antibiotics under low,medium,and high levels of spiking were 90.9%to 108.7%,with a relative standard deviation of 2.1%to 9.4%.Compared with the traditional solid-phase extraction purification method,this detection method with POP had the characteristics of operation convenience,energy-saving,and high efficiency,and with good repeatability and high recovery rate,it can be used for the detection of various antibiotic residues in honey.
作者
王安琪
张斌骏
秦宇
张申平
WANG Anqi;ZHANG Binjun;QIN Yu;ZHANG Shenping(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 200233;School ofBiotechnology,East China University Of Science and Technology,Shanghai 200237)
出处
《中国食品添加剂》
CAS
2024年第6期193-202,共10页
China Food Additives
基金
上海市质量监督检验技术研究院项目(KY-2020-9-SP)。
关键词
超交联聚合物材料
合成方法
抗生素残留检测
蜂蜜
hypercrosslinked polymer
synthetic method
antibiotics residues detection
honey
