水产品及其苗种中硝基呋喃代谢物的高效液相色谱- 串联质谱法测定

doi:10.7506/spkx1002-6630-201012048

食品科学 ›› 2010, Vol. 31 ›› Issue (12): 206-211.doi: 10.7506/spkx1002-6630-201012048

水产品及其苗种中硝基呋喃代谢物的高效液相色谱- 串联质谱法测定

杨琳¹，傅红²，刘强²

1.福建省海洋环境与渔业资源监测中心 2.福州大学生物科学与工程学院

收稿日期:2009-09-04 修回日期:2010-03-17 出版日期:2010-06-15 发布日期:2010-12-29
通讯作者: 傅红 E-mail:fuhong7766@gmail.com

Determination of Nitrofuran Metabolites in Fish and Fry Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

YANG Lin1，FU Hong2，LIU Qiang2

1. Fujian Provincal Monitor Center of Ocean Environment and Fish Source, Fuzhou 350003, China ；
2. College of Biological Science and Technology, Fuzhou University, Fuzhou 350108, China

Received:2009-09-04 Revised:2010-03-17 Online:2010-06-15 Published:2010-12-29
Contact: FU Hong E-mail:fuhong7766@gmail.com

摘要/Abstract

摘要：

对115 个水产品及鱼苗样品进行呋喃妥因(AHD)、呋喃它酮(AMOZ)、呋喃唑酮(AOZ)和呋喃西林(SEM)4 种硝基呋喃代谢物残留量分析。样品水解、衍生和净化后，采用液相色谱- 电喷雾三重四级杆串联质谱仪检测，多反应监测扫描模式和同位素内标法定量。各类硝基呋喃代谢物线性范围为0.5～20ng/mL、检出限0.25μg/kg，在0.25～5μg/kg 范围内样品添加回收率为89.0%～117.2%，相对标准偏差小于10%。结果表明，水产鱼苗中的硝基呋喃代谢物残留量远远高于成鱼，其中大黄鱼苗中AOZ 的检出率为62%，最大残留量3890μg/kg，而大黄鱼成鱼AOZ 的检出率17%，最大残留量2.81μg/kg，同时淡水鱼的硝基呋喃类药物残留小于海产鱼。

关键词: 硝基呋喃代谢物, 高效液相色谱- 串联质谱, 水产品

Abstract:

In this study, we presented a high performance liquid chromatography-tandem mass spectrometric (HPLC-MS/MS) method for determining 4 nitrofuran metabolites in 115 fish or fry products, namely 1-aminohydantoin hydrochloride (AHD), 3-amino-5-morpholinomethyl-2-oxazolidineone (AMOZ), 3-amino-2- oxazolidinone (AOZ) and semicarbazide (SEM). Samples were subjected to hydrolysis, derivation and clean-up prior to HPLC-MS/MS analysis. The analysis was carried out in the multi reaction monitoring (MRM) mode and internal standard isotope dilution method was used for quantification. Calibration curves for the analytes exhibited good linearity over the concentration range from 0.5 to 20 ng/mL and their limits of detection were all 0.25μg/kg. Average recoveries for them spiked at 3 levels ranged from 89.0% to 117.2%, with a RSD of less than 10%. Nitrofuran metabolites residues in fry were found much higher than those in adult fish. The detection rate of AOZ in large yellow croaker fry was 62%, with a maximum residue of 3890μg/kg; however, for large yellow croaker, the detection rate and the maximum residue were both comparatively lower, 17% and 2.81μg/kg, respectively. Less nitrofuran metabolites residues were detected in fresh water fish than in their sea counterpart.

Key words: nitrofuran metabolites, high performance liquid chromatography-tandem mass spectrometry, fish and fry products

中图分类号:

TS254.7

杨琳1，傅红2，刘强2. 水产品及其苗种中硝基呋喃代谢物的高效液相色谱- 串联质谱法测定[J]. 食品科学, 2010, 31(12): 206-211.

YANG Lin1，FU Hong2，LIU Qiang2. Determination of Nitrofuran Metabolites in Fish and Fry Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, 2010, 31(12): 206-211.

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水产品及其苗种中硝基呋喃代谢物的高效液相色谱- 串联质谱法测定

Determination of Nitrofuran Metabolites in Fish and Fry Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

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