食品科学 ›› 2018, Vol. 39 ›› Issue (20): 337-343.doi: 10.7506/spkx1002-6630-201820049

• 安全检测 • 上一篇    

超高效液相色谱-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1,3,黄东仁2   

  1. (1.福州大学生物科学与工程学院,福建?福州 350108;2.福建省海洋环境与渔业资源监测中心,福建?福州 350003;3.福州大学?福建省海洋酶工程重点实验室,福建?福州 350108)
  • 出版日期:2018-10-25 发布日期:2018-10-24
  • 基金资助:
    福建省科技计划社会发展引导性项目(2016Y0004); 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(2016fjscq01)

Rapid Screening of 16 Hormone Residues in Aquatic Products by Ultra Performance Liquid Chromatography Coupled with Quadrupole Time-of-Flight Mass Spectrometry

CHEN Qiuhua1, ZHANG Tianwen2,*, FU Hong1,3, HUANG Dongren2   

  1. (1. College of Biological Science and Technology, Fuzhou University, Fuzhou 350108, China; 2. Fujian Marine Environment and Fishery Resources Monitoring Center, Fuzhou 350003, China; 3. Fujian Provincial Key Laboratory of Marine Enzyme Engineering, Fuzhou University, Fuzhou 350108, China)
  • Online:2018-10-25 Published:2018-10-24

摘要: 建立改良的QuEChERS前处理方法,结合超高效液相色谱-四极杆飞行时间质谱快速筛查水产品中16?种激素残留。样品均质后经体积分数1%乙酸-乙腈提取,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%甲酸溶液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1~100?μg/L范围内线性关系良好,相关系数(r2)为0.990?6~0.999?9,4?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%,相对标准偏差为0.93%~10.9%。方法检出限为0.2~2.7?μg/kg,方法定量限为0.8~8.2?μg/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 a modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) combined with ultra performance liquid chromatography-quadrupole time of flight mass spectrometry (UPLC-Q-TOF MS). The homogenized samples were extracted with acetonitrile containing 1% acetic acid, and the extract was desalted with sodium chloride and anhydrous magnesium sulfate, defatted with n-hexane and then cleaned-up on a C18 column. The analytes were separated on a BEH C18 column using a mixture of 0.1% formic acid and methanol as mobile phase by gradient elution and analyzed by MS using electrospray ionization (ESI) in positive ionization mode. The linear range was 1–100 μg/L for all compounds with correlation coefficients of more than 0.990 6. The recoveries of the hormones at three different spiked levels ranged from 53.6% to 135.2%, with relative standard deviations (RSDs) of 0.93% to 10.9% in Penaeus vannamei, Pseudosciaena crocea, grass carp and swimming crab matrices. The limits of detection (LODs) (RSN = 3) were in the range of 0.2–2.7 μg/kg and the limits of quantification (LOQs) (RSN = 10) for the analytes were 0.8–8.2 μg/kg. The method is simple, rapid, accurate and suitable for rapid screening of hormones in aquatic products samples.

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

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