新型QuEChERS方法结合高效液相色谱串联四极杆飞行时间质谱法快速测定鱼肉中14种激素  

Simultaneous determination of fourteen hormones in fish meat by liquid chromatography/quadrupole time-of-flight mass spectrometry combined with novel QuEChERS method

作　　者：李诗言[1] 王扬[1] 周凡[1] 郑重莺 柯庆青 王鼎南 贝亦江[1] LI Shiyan WANG Yang ZHOU Fan ZHENG Chongying KE Qingqing WANG Dingnan BEI Yijiang(Aquatic Products Quality Inspection Center of Zhejiang Province, Hangzhou 310023, China)

机构地区：[1]浙江省水产质量检测中心,浙江杭州310023

出　　处：《中国渔业质量与标准》2016年第5期52-59,共8页Chinese Fishery Quality and Standards

基　　金：资助项目:浙江省2013年农业标准化研究

摘　　要：建立了一种新型QuEChERS前处理方法,结合高效液相色谱-四极杆飞行时间质谱（LC-Q-TOF/MS）技术对鱼肉中14种激素进行快速筛查测定。样品加入水分散基质后采用乙腈提取,提取液经增强型基质去脂吸附剂（EMRlipid）脱脂,盐析后采用PSA吸附剂进一步净化并浓缩,然后用LC-Q-TOF/MS方法检测分析。所有药物在线性范围内线性良好,定量限范围为1.4-6.7μg/kg。3个添加水平（n=6）下草鱼基质的平均回收率为75.4%-103.6%,相对标准偏差（RSD）为2.4%-9.5%;大黄鱼基质的平均回收率为73.4%-101.5%,相对标准偏差（RSD）为2.4%-9.1%。该方法利用精确质量数匹配和自建标准谱库检索,实现快速筛查,并使用多级特征碎片离子进行确证,具有操作简便、结果准确等优点,适用于不同鱼肉基质,可作为鱼肉中14种激素类药物的高通量筛查和确认检测方法。本研究为监测鱼肉中激素类药物的风险提供了有效的技术手段。The novel QuEChERS sample preparation and liquid chromatography/quadrupole time-of-flight mass spec- trometry （LC-Q-TOF/MS） method was developed for the determination of 14 hormones in fish meat. The homogenized sample was dispersed by water, and then the analytes were extracted by acetonitrile. The extraction was degreased by enhanced matrix removal （EMR-lipid） material. After the sahing-out, PSA adsorbent was used for further purificationand concentration. Then, the analytes were detected by liquid chromatography/quadrupole time-of-flight mass spec- trometry （LC-Q-TOF/MS）. The linear ranges of the analytes were good within the linearity range, and the limits of detection （LOD） were from 1.4 to 6.7 μg/kg. At the different spiked levels （ n = 6）, the average recoveries were from 75.4% to 103.6% and the relative standard deviations （RSD） ranged from 2.4% to 9.5% in the Grass carp （Ctenopharyngodon idellus） meat; the average recoveries were from 73.4% to 101.5% and the relative standard de- viations （RSD） ranged from 2.4% to 9.1% in the Pseudosciaena crocea（Larimichthys crocea）meat. The screening of analytes was performed by precision mass matching and library search. This proposed method was convenient, reliable and simple. The method was also suitable for the rapid screening analysis of 14 hormones in fish meat as a high- throughput and confirmatory method. This research provided an effective technical means for monitoring the risk of hor- mones in fish.

关 键 词：高效液相色谱串联四极杆飞行时间质谱 激素 QUECHERS 草鱼 大黄鱼 筛查参数 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]