摘要
目的建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)定量检测水产品苗种中氯霉素残留的分析方法。方法以三疣梭子蟹苗种、中国对虾苗种、半滑舌鳎苗种、海参苗种、菲律宾蛤仔苗种为实验基质进行加标,经乙酸乙酯提取、正己烷/N-丙基乙二胺(N-propylenediamine,PSA)净化后取下层清液过滤膜,进行检测。采用ACQUITY UPLCBEHC C_(18)色谱柱(100 mm×2.1 mm,1.7μm);柱温30℃;采用梯度洗脱方式,流动相分别为水和乙腈;进样量2μL。结果氯霉素检出限为0.15μg/kg,定量限为0.30μg/kg。在0.15~10.00 ng/mL质量浓度范围内,线性关系良好,相关系数为0.9993。5倍加标平均回收率在84.6%~95.3%之间,相对标准偏差在2.43%~5.12%之间,整体不确定度为±10.3%。结论该方法操作简单、灵敏度高、重现性好,可以满足水产品苗种中氯霉素残留的检测要求。
Objective To establish method for the quantitative determination of chloramphenicol residues in aquaculture fry by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods Portunus trituberculatus,Fenneropenaeus chinensis,Cynoglossus semilaevis,sea cucumbers and Ruditapes philippinarum were used as experimental substrates for labeling.After extraction with ethyl acetate and purification with n-hexane/N-propylethylenediamine(PSA),the lower clear liquid was filtered through a membrane for detection.ACQUITY UPLCBEHC C_(18) chromatographic column(100 mm×2.1 mm,1.7μm)was used;column temperature was 30℃;the gradient elution method was adopted,with water and acetonitrile as the mobile phases;injection volume was 2μL.Results The limit of detection of chloramphenicol was 0.15μg/kg,and the limit of quantitation was 0.30μg/kg.The linear relationship was good within the mass concentration range of 0.15-10.00 ng/mL,with a correlation coefficient of 0.9993.The average recovery rates of 5-fold spiked samples were between 84.6%and 95.3%,the relative standard deviations were between 2.43%and 5.12%,and the overall uncertainty was±10.3%.Conclusion The method is simple,rapid,accurate and reliable,and suitable for the rapid screening of chloramphenicos in aquaculture fry residues.
作者
王景
薛敬林
罗晶晶
丁玉竹
王明磊
崔庆奎
孙琰晴
韩典峰
WANG Jing;XUE Jing-Lin;LUO Jing-Jing;DING Yu-Zhu;WANG Ming-Lei;CUI Qing-Kui;SUN Yan-Qing;HAN Dian-Feng(Shandong Marine Resources and Environment Research Institute,Yantai 264006,China)
出处
《食品安全质量检测学报》
2025年第24期236-242,共7页
Journal of Food Safety and Quality
基金
山东省现代农业产业技术体系项目(SDAIT-14-08,SDAIT-22-08,SDAIT-26-05)。
关键词
氯霉素
水产品苗种
高效液相色谱-串联质谱法
chloramphenicol
aquaculture fry
high performance liquid chromatography-tandem mass spectrometry
