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当前位置: 首页 > 文章 > 分散固相萃取净化-液相色谱-质谱联用测定水产苗种中硝基呋喃类代谢物残留量 食品科学 2014,35 (16) 153-159
Position: Home > Articles > Determination of Nitrofuran Metabolite Residues in Aquatic Fingerlings by High Performance Liquid Chromatography-Mass Spectrometry with Dispersive Solid Phase Extraction FOOD SCIENCE 2014,35 (16) 153-159

分散固相萃取净化-液相色谱-质谱联用测定水产苗种中硝基呋喃类代谢物残留量

作  者：
严忠雍;张小军;梅光明;李佩佩;龙举;祝银;王建
单  位：
浙江工商大学食品与生物工程学院;浙江省海洋水产研究所
关键词：
分散固相萃取;液相色谱-质谱;水产苗种;硝基呋喃类代谢物
摘  要：
建立分散固相萃取净化-液相色谱-质谱法测定水产苗种中氨基脲、5-甲基吗啉-3-氨基-2-噁唑烷基酮、3-氨基-2-噁唑烷基酮、1-氨基-2-内酰脲,4种硝基呋喃类代谢物残留量的方法。样品经甲醇-水(8:1,v/v)溶液洗涤后,盐酸溶液水解,以2-硝基苯甲醛作为衍生化试剂,乙酸乙酯萃取,浓缩,分散固相萃取净化,采用液相色谱-质谱仪、多反应监测扫描模式检测和同位素内标定量。4种硝基呋喃类代谢物在0.5~20 μg/L范围内线性相关系数大于0.997,检出限0.1 μg/kg,回收率90.5%~104.5%,相对标准偏差1.56%~8.08%。本方法灵敏、高效、简单、重复性好,满足硝基呋喃类代谢物的检测要求。
译  名：
Determination of Nitrofuran Metabolite Residues in Aquatic Fingerlings by High Performance Liquid Chromatography-Mass Spectrometry with Dispersive Solid Phase Extraction
作  者：
YAN Zhong-yong;ZHANG Xiao-jun;MEI Guang-ming;LI Pei-pei;LONG Ju;ZHU Yin;WANG Jian;Marine Fisheries Research lnstitute of Zhejiang Province;Key Laboratory of Sustainable Utilization of Technology Research for Fishery Resourceof Zhejiang Province;College of Food Science and Biotechnology, Zhejiang Gongshang University;
关键词：
dispersive solid phase extraction;;high performance liquid chromatography-mass spectrometry;;aquatic fingerlings;;nitrofuran metabolites
摘  要：
A method has been developed for the determination of four metabolites of nitrofuran, i.e. semicarbazide(SEM), 3-amino-5-morpholinomethyl-2-oxazolidineone (AMOZ), 3-amino-2-oxazolidinone (AOZ) and 1-aminohydantoin hydrochloride (AHD) in aquatic fingerlings, by high performance liquid chromatography-mass spectrometry with dispersive solid phase extraction. Samples were washed with a mixture of methanol-water(8:1, v/v), subjected to HCl acidolysis and derivatized using 2-nitrobenzaldehyde. The derivative was extracted with ethyl acetate, then concentrated and cleaned up by dispersive solid phase extraction. The analysis was carried out in the multi-reaction monitoring (MRM) mode and internal standard isotope dilution method was used for quantification. Good linearity was obtained in the correlations between the peak areas and concentrations of the four metabolites of nitrofuran antibiotics over the concentration range from 0.5 to 20.0 μg/L, with correlation coefficients above 0.997. The limits of detection (LODs) for the four compounds were all 0.1 μg/kg. The range of average recoveries was between 90.5% and 104.5%, with relative standard deviations (RSDs) between 1.56% and 8.08%. The efficient and simple method could be used to identify and quantify the metabolites of nitrofuran antibiotics in aquatic fingerlings with satisfactory sensitivity and repeatability.

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