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浙江大学学报(理学版)  2017, Vol. 44 Issue (3): 339-344    DOI: 10.3785/j.issn.1008-9497.2017.03.015
环境科学     
QuEChERS-超高效液相色谱串联质谱法测定水产品中红霉素残留
严忠雍1,2, 张小军1,2, 李佩佩1,2, 方益1,2, 喻亮1,2, 张帅1,2, 祝银1,2, 李强3
1. 浙江省海洋水产研究所, 浙江 舟山 316021;
2. 浙江省海洋渔业资源可持续利用技术研究重点实验室, 浙江 舟山 316021;
3. 中国水产科学研究院, 北京 100141
QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry for the determination of erythromycin in fishy products
YAN Zhongyong1,2, ZHANG Xiaojun1,2, LI Peipei1,2, FANG Yi1,2, YU Liang1,2, ZHANG Shuai1,2, ZHU Yin1,2, LI Qiang3
1. Marine Fisheries Research Institute of Zhejiang, Zhoushan 316021, Zhejiang Province, China;
2. Key Lab of Sustainable Utilization of Technology Research for Fishery Resource of Zhejiang, Zhoushan 316021, Zhejiang Province, China;
3. Chinese Academy of Fishery Sciences, Beijing 100141, China
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摘要: 建立了超高效液相色谱串联质谱法测定水产品中的红霉素残留量.样品用改进的QuEChERS(快速、简单、廉价、高效、灵活和安全)进行提取净化,经乙腈快速提取,无水硫酸镁和氯化钠除水后,用N-丙基乙二胺(PSA)净化,液相色谱串联质谱分析测定.在ACQUITY UPLC BEH C18色谱柱上进行分离,采用梯度洗脱,以0.1%甲酸水溶液和甲醇为流动相,电喷雾正离子电离,多反应监测模式,内标法定量.结果表明:红霉素浓度在0.5~50 μg·L-1时具有良好的线性关系,相关系数为0.997 6,定量限为0.3 μg·kg-1,回收率为87.6%~96.1%,相对标准偏差为2.2%~5.3%.本方法操作简易、应用性强,适合水产品中红霉素的常规检测.
关键词: QuEChERS液相色谱串联质谱水产品红霉素    
Abstract: A method has been developed for the determination of erythromycin in fishery products by ultra performance liquid chromatography-tandem mass spectrometry. The samples were pretreated using the modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) method that completed the extraction and clean-up steps in one procedure. The samples were extracted with acetonitrile, dehydrated with sodium chloride and anhydrous magnesium sulfate, and cleaned up by dispersive solid phase extraction on primary secondary amine, and then were detected by HPLC-MS/MS. The chromatographic separation was performed on an ACQUITY UPLC BEH C18 column by gradient elution using methanol and 0.1% formic acid solution as mobile phase. Internal standard method was used for quantification, and the positive electrospray ionization source was applied under the multiple reaction monitoring mode. Linear ranges of erythromycin was in the range of 0.5 to 50.0 μg·L-1 with correlation coefficient of 0.997 6. The quantification limit of the method was 0.3 μg·kg-1. The recoveries of erythromycin were from 87.6% to 96.1%, and the relative standard deviation was from 2.2% to 5.3%. The method was simple, fast and sensitive for the analysis of erythromycin in fishy products.
Key words: QuEChERS    high performance liquid chromatography-tandem mass spectrometry    fishy products    erythromycin
收稿日期: 2016-01-29 出版日期: 2017-03-01
CLC:  O657.6  
基金资助: 公益性行业(农业)科研专项(201503108);浙江省公益性技术研究项目(2014C32087).
通讯作者: 张小军,ORCID:http://orcid.org/0000-0001-8807-5450,E-mail:xiaojun3627@163.com.     E-mail: xiaojun3627@163.com
作者简介: 严忠雍(1990-),ORCID:http://orcid.org/0000-0002-3147-3738,男,学士,主要从事水产品质量安全与渔业环境监测.
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引用本文:

严忠雍, 张小军, 李佩佩, 方益, 喻亮, 张帅, 祝银, 李强. QuEChERS-超高效液相色谱串联质谱法测定水产品中红霉素残留[J]. 浙江大学学报(理学版), 2017, 44(3): 339-344.

YAN Zhongyong, ZHANG Xiaojun, LI Peipei, FANG Yi, YU Liang, ZHANG Shuai, ZHU Yin, LI Qiang. QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry for the determination of erythromycin in fishy products. Journal of Zhejiang University (Science Edition), 2017, 44(3): 339-344.

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https://www.zjujournals.com/sci/CN/10.3785/j.issn.1008-9497.2017.03.015        https://www.zjujournals.com/sci/CN/Y2017/V44/I3/339

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