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。
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
所属栏目 工作简报
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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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【6】赵东豪,黎智广,王旭峰,等.高效液相色谱-串联质谱法检测水产品中硝基呋喃类代谢物的优化研究[J].南方水产科学, 2015,11(6):58-64.
【7】孙稚菁,王婵,李崇,等.高效液相色谱-串联质谱法快速检测海参中硝基呋喃代谢物前处理方案的探讨[J].分析测试学报, 2016,35(9):1127-1131.
【8】包永华,王璐璐.超高效液相色谱-串联四极杆质谱法测定水产品中硝基呋喃类代谢物的方法改进[J].中国兽药杂志, 2019,53(9):27-33.
【9】宋瑞,李云,赵义良,等.国家标准方法测定水产品中硝基呋喃类代谢物残留量检测方法的改进[J].中国兽药杂志, 2019,53(9):57-64.
【2】傅国,李宁毅.硝基呋喃类和硝基咪唑类药物的研究进展[J].青岛大学医学院学报, 2003,39(4):486-488.
【3】LAURENSEN J J, NOUWS J F M. Simultaneous determination of nitrofuran derivatives in various animal substrates by high-performance liquid chromatography[J]. Journal of Chromatography A, 1989,472:321-326.
【4】YNDESTAD M. Public health aspects of residues in animal products:Fundamental considerations[M]. Oslo:Norwegian College of Veterinary Medicine, 1990.
【5】唐红梅,曾芳,李成洪.食品中硝基呋喃类药物及其代谢物残留检测的研究进展[J].食品安全质量检测学报, 2016,7(10):3952-3959.
【6】赵东豪,黎智广,王旭峰,等.高效液相色谱-串联质谱法检测水产品中硝基呋喃类代谢物的优化研究[J].南方水产科学, 2015,11(6):58-64.
【7】孙稚菁,王婵,李崇,等.高效液相色谱-串联质谱法快速检测海参中硝基呋喃代谢物前处理方案的探讨[J].分析测试学报, 2016,35(9):1127-1131.
【8】包永华,王璐璐.超高效液相色谱-串联四极杆质谱法测定水产品中硝基呋喃类代谢物的方法改进[J].中国兽药杂志, 2019,53(9):27-33.
【9】宋瑞,李云,赵义良,等.国家标准方法测定水产品中硝基呋喃类代谢物残留量检测方法的改进[J].中国兽药杂志, 2019,53(9):57-64.
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