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• 安全检测 •    下一篇

液相色谱-四极杆飞行时间质谱法快速筛查水产品中16种激素残留

陈秋华1,张天闻2,傅红1,黄东仁2   

  1. 1. 福州大学生物科学与工程学院
    2. 福建省海洋环境与渔业资源监测中心
  • 收稿日期:2017-10-18 修回日期:2018-07-24 出版日期:2018-10-25 发布日期:2018-10-24
  • 通讯作者: 张天闻 E-mail:zhangtw1986@163.com
  • 基金资助:
    福建省科技计划社会发展引导性项目;福建省海洋生物增养殖与高值化利用重点实验室开放课题资助项目

Rapid screening of 16 hormone residues in aquatic products by liquid chromatography coupled with quadrupole time-of-flight mass spectrometry

1,Tianwen ZHANG 1, 1   

  • Received:2017-10-18 Revised:2018-07-24 Online:2018-10-25 Published:2018-10-24
  • Contact: Tianwen ZHANG E-mail:zhangtw1986@163.com

摘要: 建立了改良的QuEChERS前处理方法,结合超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF/MS)快速筛查水产品中16种激素残留。样品均质后经1%乙酸-乙腈(v:v)提取,氯化钠和无水硫酸镁盐析,正己烷脱脂和十八烷基键合硅胶吸附剂(C18)净化后,采用BEH C18色谱柱分离,以0.1%甲酸水(v:v)和甲醇为流动相进行梯度洗脱,电喷雾正离子模式检测。16种激素在1~100μg/L范围内线性关系良好,相关系数(r2)为0.9906~0.9999,4种不同水产品(南美白对虾、大黄鱼、梭子蟹、草鱼)在3个添加水平下,回收率为53.6%~135.2%,相对标准偏差(RSD)为0.93%~10.9%。方法检出限(S/N=3)为0.2~2.7μg/kg, 方法定量限(S/N=10)为0.8~8.2μg/kg。建立的方法快速、准确,适用于水产品中激素的快速筛查。

关键词: 超高效液相色谱-四极杆飞行时间质谱, 水产品, QuEChERS, 激素

Abstract: An analytical method was established for rapid screening of 16 hormone residues in aquatic product by modified QuECHERS combined with ultra performance liquid Chromatography-quadrupole time of flight mass spectrometry (UPLC-QTOF-MS).The homogenized sample were extracted with 1% acetic acid acetonitrile,salting out with sodium chloride and anhydrous magnesium sulfate,and defatted with n-hexane,then cleaned-up by C18.Analysis were separated on an BEH C18 column using water with 0.1% formic acid and methanol as mobile phase by gradient,analyzed by MS under ESI positive ionization mode.The linear range was 1~100μg/L for each compound with the correlation coefficients of more than 0.9906. At the different spiked level,the recoveries were ranged from 53.6% to 135.2%,with relative standard deviations (RSDs) ranged from 0.93% to10.93% in Penaeus vannamei,Pseudosciaena crocea,Grass Carp and Swimming crab matrices。The limits of detection (LODs) (S/N=3) were 0.2~2.7μg/kg and the limits of quantification (LOQs) (S/N=10) for the analytes were 0.8~9.0μg/kg. The method is simple, rapid and accurate for rapid screening of hormones in aquatic products samples.

Key words: ultra performance liquid Chromatography-quadrupole time of flight mass spectrometry (UPLC-QTOF-MS), aquatic product, QuEChERS, hormones

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