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HPLC-MS/MS检测禽蛋中赛红霉素残留量的方法建立
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作者单位:

1.中华人民共和国聊城海关，山东 聊城 252027;2.济南海关技术中心，山东 济南 250002;3.上海海关动植物与食品检验检疫技术中心，上海 200135;4.青岛海关技术中心，山东 青岛 266114;5.中华人民共和国黄岛 海关，山东 青岛 266300;6.中华人民共和国枣庄海关，山东 枣庄 277020;7.中华人民共和国潍坊海关，山东 潍坊 261031

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通讯作者:

王乐（1982—），女，博士，研究员，主要从事农产品质量安全检测研究。E-mail：183825851@qq.com

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基金项目:

国家“十四五”重点研发计划项目（2022YFF1100802）；海关技术规范计划项目（2023B228）；聊城市重点研发计划政策引导类项目（2024YD09）。


Establishment of a HPLC-MS/MS Method for Determination of Cethromycin Residue in Poultry Eggs
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Affiliation:

1.Liaocheng Customs of the People’s Republic of China, Liaocheng 252027, China;2.Technology Center of Jinan Customs, Jinan 250002, China;3.Animal, Plant and Food Inspection and Quarantine Technology Center of Shanghai Customs, Shanghai 200135, China;4.Technology Center of Qingdao Customs, Qingdao 266114, China;5.Huangdao Customs of the People’s Republic of China, Qingdao 266300, China;6.Zaozhuang Customs of the People’s Republic of China, Zaozhuang 277020, China;7.Weifang Customs of the People’s Republic of China, Weifang 261031, China

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    摘要:

    【目的】建立一种适用于禽蛋中赛红霉素残留量检测的高效液相色谱-串联质谱（high performance liquid chromatography-tandem mass spectrometry，HPLC-MS/MS）方法。【方法】选取鸡蛋、鸭蛋、鹅蛋、鹌鹑蛋这4种禽蛋为研究基质，以Mcllvaine-Na2EDTA缓冲液为提取溶剂，经亲水亲脂共平衡聚合物固相萃取（HLB）柱净化，以含体积分数0.1%甲酸的水溶液和乙腈为流动相，以C18色谱柱为固定相，采用多反应监测（MRM）模式结合HPLC-MS/MS外标法进行赛红霉素残留量测定。【结果】赛红霉素在色谱柱上分离效果良好， 标准曲线在1~100 μg/kg的线性关系良好（R2≥0.999）， 检测限（LOD）为0.3 μg/kg，定量限（LOQ）为1.0 μg/kg；加标回收率为76.3%~102.6%，相对标准偏差（RSD）均小于15%（n=6）。【结论】该方法操作简单、定性及定量准确，适用于禽蛋中赛红霉素残留量的快速筛查与定量分析。

    Abstract:

    [Objective] This study aims to establish a method for determining the residual amount of cethromycin in poultry eggs based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).[Method] Four representative poultry eggs (chicken eggs, duck eggs, goose eggs, and quail eggs) were selected as the research matrices. Cethromycin was extracted with Mcllvaine-Na2EDTA buffer solution, purified by hydrophilic-lipophilic balanced polymer solid-phase extraction column (HLB), separated by a C18 column with 0.1% (volume fraction) formic acid water and acetonitrile as the mobile phase, and determined by HPLC-MS/MS in the multiple reaction monitoring (MRM) mode combined with an external standard method.[Result] Cethromycin was well separated on the chromatographic column. The standard curve had a good linear relationship (R2≥0.999) in the range of 1~100 μg/kg. The limit of detection (LOD) was 0.3 μg/kg, and the limit of quantification (LOQ) was 1.0 μg/kg. The spiked recovery rates ranged from 76.3% to 102.6%, and the relative standard deviations (RSD) were all less than 15% (n=6).[Conclusion] The established method is simple to operate and accurate in qualitative and quantitative analyses. It can be used for the rapid screening and quantitative analysis of cethromycin in poultry eggs.

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常晨阳,王粮子,王乐,常凯,单娇,王晓,郭礼强. HPLC-MS/MS检测禽蛋中赛红霉素残留量的方法建立[J].食品与生物技术学报,2025,44(8):41-48.

CHANG Chenyang, WANG Liangzi, WANG Le, CHANG Kai, SHAN Jiao, WANG Xiao, GUO Liqiang. Establishment of a HPLC-MS/MS Method for Determination of Cethromycin Residue in Poultry Eggs[J]. Journal of Food Science and Biotechnology,2025,44(8):41-48.

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  • 收稿日期:2024-09-14
  • 最后修改日期:2024-11-05
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  • 在线发布日期: 2025-11-26
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