摘要
建立了QuEChERS-高效液相色谱-串联质谱同时检测奶粉中玉米赤霉烯酮及其代谢产物的检测方法。样品用10 mL超纯水溶解,1%乙酸乙腈溶液提取,乙酸钠盐析,C18、N-丙基乙二胺(primary secondary amine,PSA)和无水硫酸镁净化,在ZORBAX SB-C18色谱柱上分离,以5 mmol/L乙酸铵溶液和乙腈作为流动相进行梯度洗脱,ESI负离子模式扫描,多反应监测(MRM)测定,β-玉米赤霉烯醇内标法定量分析。奶粉中玉米赤霉烯酮及其代谢产物在0.1~50μg/L浓度范围内呈线性关系,相关系数均高于0.999,基质效应为抑制效应;检出限(LOD)均为0.1μg/kg,定量限(LOQ)均为0.2μg/kg。奶粉中玉米赤霉烯酮及其代谢产物的3个加标浓度水平的平均回收率范围为85.2%~119.3%,相对标准偏差(RSD)在0.3%~12.2%(n=7)之间。该方法简便快速、准确可靠,可用于检测奶粉中玉米赤霉烯酮及其代谢物。
A method for simultaneous determination of zearalenone and its metabolites(ZERs)in milk powder was developed by high performance liquid chromatography-tandem mass spectrometry with QuEChERS cleanup.The sample was diluted with 10 mL ultra-pure water,extracted by 1%acetonitrile acetate,and sodium acetate salting out,cleaned up with C18,PSA and mgnesium sulfate anhydrous.The analytes were separated by a reversed phase C18 column and gradiently eluted with 5 mmol/L ammonium acetate and acetonitrile.The determination was conducted by negative electrospray ionization(ESI-)with the multiple reaction monitoring(MRM)mode.The ZERs was quantified by internal standard method withβ-zearalenol-d7.The good linearities were obtained for ZERs at the concentration of 0.1~50μg/L with the linear correlation coefficients more than 0.999,and the matrix effect was inhibition.The limits of detection(LOD)and the limits of quantification(LOQ)for ZERs were 0.1μg/kg and 0.2μg/kg,respectively.The recoveries at three concentration spiked levels were in the range of 85.2%~119.3%.The repeatability expressed as relative standard deviations(RSD)was ranged from 0.3%to 12.2%(n=7).The method is simple,rapid,accurate and reliable,and can be used for detecting ZERs in milk powder.
作者
谢瑜杰
陈辉
胡雪艳
刘志楠
范春林
呼秀智
彭涛
XIE Yu-jie;CHEN Hui;HU Xue-yan;LIU Zhi-nan;FAN Chun-lin;HU Xiu-zhi;PENG Tao(Chinese Academy of Inspection and Quarantine,Beijing 100176,China;College of Life Science and Food Engineering,Hebei University of Engineering,Handan 056021,China)
出处
《食品工业科技》
CAS
北大核心
2020年第7期233-238,共6页
Science and Technology of Food Industry
基金
特色高值农产品新型甄别检测关键技术研究(2017YFF0211300)。
关键词
奶粉
玉米赤霉烯酮
QUECHERS
高效液相色谱-串联质谱
milk powder
zearalenone and its metabolites
QuEChERs
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
作者简介
谢瑜杰(1994-),女,硕士研究生,研究方向:食品安全检测,E-mail:1443908316@qq.com;通讯作者:彭涛(1976-),男,博士,研究员,研究方向:兽药残留分析,食品安全研究,E-mail:caiq_pengtao@126.com。
