摘要
基于糖析萃取/超高效液相色谱-四极杆/静电场轨道阱高分辨质谱技术,建立了蜂蜜中68种化学风险物质的分析方法。蜂蜜样品提取液经色谱柱分离,进入四极杆/静电场轨道阱高分辨质谱进行数据采集。通过对比样品与标准品一级质谱分子离子精确质量数、保留时间、同位素丰度比对所得数据进行初筛;初筛得到的阳性化合物采用二级碎片离子进一步确证。该方法实现了蜂蜜中68种风险物质的同时精准筛查,目标风险物质的检出限为0.03~2.73µg/kg,定量下限为0.10~9.00µg/kg,平均加标回收率为50.7%~122%,相对标准偏差为1.0%~15%。采用所建立的方法对32份市售蜂蜜样品进行检测,在12份样品中检出蝇毒磷,检出含量范围为0.74~24.87µg/kg。该方法通量高、速度快、定量准确,可用于蜂蜜中风险物质的快速筛查。
An analytical method for detection of 68 chemical risk substances in honey was estab-lished based on sugar extraction/ultra high performance liquid chromatography-quadrupole/electro-static field orbitrap high resolution mass spectrometry technology.The honey extracts were separated by a chromatographic column and then analyzed by quadrupole electrostatic field orbitrap high resolu-tion mass spectrometry.The acquired sample information and the standard information were prelimi-nary screening through the accurate mass number,retention time and isotope distribution ratio com-parison.The positive compounds in the initial screening were further confirmed by comparing the sec-ondary fragment ions.This method can accurately screen 68 risk substances in honey within 17 min-utes,with the detection limits of 0.03-2.73µg/kg,the quantification limits of 0.10-9.00µg/kg,the recoveries of 50.7%-122%and the relative standard deviations(RSDs)of 1.0%-15%.This meth-od was used to detect 32 honey samples,and coumaphos was detected in 12 samples,with the detec-tion concentration ranging from 0.74 to 24.87µg/kg.This method has high throughput,fast speed,and accurate quantification,and can be used for rapid screening of risk substances in honey.
作者
高佳
刘梦颖
任贝贝
路杨
陈福尊
王丽英
康维钧
GAO Jia;LIU Meng-ying;REN Bei-bei;LU Yang;CHEN Fu-zun;WANG Li-ying;KANG Wei-jun(School of Public Health,Hebei Medical University,Shijiazhuang 050017,China;Hebei Provincial Center for Disease Control and Prevention,Shijiazhuang 050021,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第10期1233-1241,共9页
Journal of Instrumental Analysis
关键词
超高效液相色谱
高分辨质谱
快速筛查
糖析萃取
蜂蜜
ultra high performance liquid chromatography(UPLC)
high resolution mass spectrom-etry
rapid screening
sugar extraction
honey
