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超高效液相色谱-串联质谱法测定动物源性食品中4种硝基呋喃类代谢物
          
UHPLC-MS/MS Determination of 4 Nitrofuran Metabolites in Animal Derived Food

摘    要
比较国家标准GB/T 20752-2006、GB/T 21311-2007以及农业部783号公告-1-2006中硝基呋喃类代谢物测定方法的优劣,确定硝基呋喃类代谢物测定的关键影响因素。动物源性食品样品不经甲醇溶液清洗,添加盐酸溶液和2-硝基苯甲醛溶液,置于37 ℃水浴中衍生反应4 h,调节pH为7.4,离心后取上清液过HLB固相萃取柱,收集洗脱液。采用超高效液相色谱-串联质谱法测定样品溶液中4种硝基呋喃类代谢物的含量。以Waters BEH C18色谱柱为固定相,以不同体积比的含2.0 mmol·L-1乙酸铵的0.05%(体积分数)甲酸溶液和2.0 mmol·L-1乙酸铵甲醇溶液的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾正离子源和多反应监测模式。采用内标法定量。4种硝基呋喃类代谢物的线性范围均为0.50~20.0 μg·L-1,检出限(3S/N)为0.05~0.25 μg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为94.0%~107%,测定值的相对标准偏差(n=6)为1.9%~3.4%。方法应用于能力验证样品(19-N866,19-P653)的分析,测定值与已知值相符。
标    签 超高效液相色谱-串联质谱法   硝基呋喃类代谢物   动物源性食品   UHPLC-MS/MS   nitrofuran metabolite   animal derived food  
 
Abstract
By comparing the advantages and disadvantages of determination methods of the nitrofuran metabolites between GB/T 20752-2006, GB/T 21311-2007 and ministry of agriculture announcement No. 783-1-2006, the key influencing factors of nitrofuran metabolites determination were determined. Hydrochloric acid solution and 2-nitrobenzaldehyde solution were added to the sample of animal derived food without washing of methanol solution, and then the sample solution was derived in water bath at 37 ℃ for 4 h. pH of the sample solution was adjusted to 7.4. After centrifugation, the supernatant was taken, and then passed through HLB solid phase extraction column. The eluate was collected. UHPLC-MS/MS was applied to the determination of 4 nitrofuran metabolites in the sample solution. Waters BEH C18 chromatographic column was used as stationary phase, and the mixture of 0.05% (volume fraction) formic acid solution containing 2.0 mmol·L-1 ammonium acetate and 2.0 mmol·L-1 ammonium acetate methanol solution mixed in different ratios was used as mobile phase in gradient elution. ESI+ and multiple reaction monitoring mode were adopted in MS/MS. Internal standard method was used for quantitative. Linearity ranges of the 4 nitrofuran metabolites were found in the same range of 0.50-20.0 μg·L-1 with detection limits (3S/N) in the range of 0.05-0.25 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 94.0%-107%, with RSDs (n=6) of determined values in the range of 1.9%-3.4%. The proposed method was applied to the analysis of proficiency testing samples (19-N866, 19-P653), giving results in consistency with the known values.

中图分类号 O657.63   DOI 10.11973/lhjy-hx202012007

 
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收稿日期 2020/1/14

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备注高海波,工程师,硕士研究生,主要从事食品理化分析与检测工作,411616817@qq.com

引用该论文: GAO Haibo,ZHANG Jinjun,LUO Zhenling. UHPLC-MS/MS Determination of 4 Nitrofuran Metabolites in Animal Derived Food[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(12): 1282~1288
高海波,张今君,罗振玲. 超高效液相色谱-串联质谱法测定动物源性食品中4种硝基呋喃类代谢物[J]. 理化检验-化学分册, 2020, 56(12): 1282~1288


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参考文献
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