液相色谱-串联质谱法测定水产品中硝呋索尔 代谢物残留量
目的 建立一种采用液相色谱-串联质谱法检测水产品中硝呋索尔代谢物残留量的测定方法。方法 样品中以结合态形式残留的硝呋索尔代谢物3,5-二硝基水杨酸肼(DNSAH)经盐酸水解, 2-硝基苯甲醛衍生, 用乙腈提取, 以电喷雾离子源负离子扫描模式进行质谱分析, 内标法定量。结果 DNSAH在0.2~20 μg/L范围内线性关系良好, 相关系数r2>0.999。DNSAH添加水平为0.50~5.00 μg/kg时, 平均回收率在88.3%~100%之间, 批内和批间变异系数均<15%。DNSAH的检出限为0.20 μg/kg。结论 本方法灵敏、高效、简单、重现性好, 满足水产品中硝呋索尔代谢物残留量的检测。
Objective To establish a method for the determination of nifursol metabolites in aquatic products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The residue of nifursol metabolite of 3,5-dinitrosalicylic acid hydrazide (DNSAH) in sample was hydrolyzed with HCl, and derivatized with nitrobenzaldehyde. Then the analyte was extracted with acetonitrile and then analyzed by HPLC-MS/MS with internal standard method. Electrospray ionization was applied and operated in the negative ion mode. Results The calibration curve had a good linearity between area and the concentration of DNSAH of 0.2~20 μg/L with the correlation coefficient over 0.999. The average recoveries from spiked sample at three concentrations of 0.50, 2.00 and 5.00 μg/kg were ranged from 88.3% to 100% with intra and inter batch relative standard deviations below 15%. The detection limit of DNSAH was 0.20 μg/kg. Conclusion The efficient and simple method can be used to identify and quantify the nifursol metabolites in aquatic products with satisfactory sensitivity and repeatability.
标题：液相色谱-串联质谱法测定水产品中硝呋索尔 代谢物残留量
英文标题：Determination of nifursol metabolites in aquatic products by high performance liquid chromatography-tandem mass spectrometry
作者：
邢丽红 中国水产科学研究院黄海水产研究所,农业部水产品质量安全检测与评价重点实验,农业部水产品质量安全风险评估实验室(青岛)
付树林 中国水产科学研究院黄海水产研究所,农业部水产品质量安全检测与评价重点实验,农业部水产品质量安全风险评估实验室(青岛)
彭吉星 中国水产科学研究院黄海水产研究所,农业部水产品质量安全检测与评价重点实验,农业部水产品质量安全风险评估实验室(青岛)
孙伟红 中国水产科学研究院黄海水产研究所,农业部水产品质量安全检测与评价重点实验,农业部水产品质量安全风险评估实验室(青岛)
郑关超 中国水产科学研究院黄海水产研究所,农业部水产品质量安全检测与评价重点实验,农业部水产品质量安全风险评估实验室(青岛)
李兆新 中国水产科学研究院黄海水产研究所,农业部水产品质量安全检测与评价重点实验,农业部水产品质量安全风险评估实验室(青岛)
翟毓秀 中国水产科学研究院黄海水产研究所,农业部水产品质量安全检测与评价重点实验,农业部水产品质量安全风险评估实验室(青岛)
中文关键词:硝呋索尔,3,5-二硝基水杨酸肼,水产品,液相色谱-串联质谱法,
英文关键词:nifursol,3,5-dinitrosalicylic acid hydrazide,aquatic products,high performance liquid chromatography- tandem mass spectrometry,
发表日期：2016-08-16
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