食品与发酵工业 >

2021 , Vol. 47 >Issue 16: 233 - 238

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.027396

分析与检测

养殖虾类中呋喃西林代谢物检测方法的优化

  • 范清涛 ,
  • 邓建朝 ,
  • 张宾 ,
  • 陈胜军 ,
  • 杨贤庆 ,
  • 李春生 ,
  • 潘创 ,
  • 王迪
展开
  • 1(浙江海洋大学 食品与药学学院,浙江 舟山,316022)
    2(中国水产科学研究院南海水产研究所,国家水产品加工技术研发中心,农业农村部水产品加工重点实验室,广东 广州,510300)
硕士研究生(陈胜军研究员为通讯作者,E-mail:chenshengjun@scsfri.ac.cn)

收稿日期: 2021-03-16

  修回日期: 2021-04-15

  网络出版日期: 2021-09-10

基金资助

国家自然科学基金(32072147);广东省重点领域研发计划资助(2019B020225001);中国水产科学研究院基本科研业务费资助(2020TD69);广东省现代农业产业技术体系创新团队建设专项资金(2021KJ151)

收起

Optimization of the detection method of furacillin metabolite residue in farmed shrimp

  • FAN Qingtao ,
  • DENG Jianchao ,
  • ZHANG Bin ,
  • CHEN Shengjun ,
  • YANG Xianqing ,
  • LI Chunsheng ,
  • PAN Chuang ,
  • WANG Di
Expand
  • 1(College of Food Science and Technology, Zhejiang Ocean University, Zhoushan 316022, China)
    2(South China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Key Laboratory of Aquatic Product Processing, Ministry of Agriculture and Rural Affairs, National R & D Center for Aquatic Product Processing, Guangzhou 510300, China)

Received date: 2021-03-16

  Revised date: 2021-04-15

  Online published: 2021-09-10

Fold

摘要

建立了微波辅助衍生结合超高效液相色谱-串联质谱快速测定养殖虾类中呋喃西林代谢物氨基脲的方法。样品经过盐酸水解,2-硝基苯甲醛微波辅助衍生,乙酸乙酯萃取,除杂净化后,采用超高效液相色谱-串联质谱法检测氨基脲含量,内标法定量。氨基脲质量浓度为0.5～100 μg/L时,线性关系良好,相关系数为0.999 6～0.999 9,检出限为0.20 μg/kg,测定结果的相对标准偏差为3.06%～6.56%,加标回收率为91.4%～103.6%。运用该方法测定了3种养殖虾类(斑节对虾、南美白对虾、罗氏沼虾)中的呋喃西林代谢物含量。该方法上机检测时间短,检出限低,具有良好的准确度和精密度,可用于虾类中氨基脲的检测。

关键词： 养殖虾; 呋喃西林; 氨基脲; 微波辅助衍生; 超高效液相色谱-串联质谱法

本文引用格式

范清涛 , 邓建朝 , 张宾 , 陈胜军 , 杨贤庆 , 李春生 , 潘创 , 王迪 . 养殖虾类中呋喃西林代谢物检测方法的优化[J]. 食品与发酵工业, 2021 , 47(16) : 233 -238 . DOI: 10.13995/j.cnki.11-1802/ts.027396

Abstract

The aim of this study was to establish a method based on microwave-assisted derivatization with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of semicarbazide (SEM) in farmed shrimp. The sample was hydrolyzed with hydrochloric acid and microwave-assisted derivatization of 2-nitrobenzaldehyde. And then it was extracted with ethyl acetate. After the purification treatment, the content of carbamide urea was determined by UPLC-MS/MS and quantified by the internal standard method. To investigate the accuracy and stability of the optimized method in different samples, standard additive experiments were carried out for different matrix samples. The results showed that, when the mass concentration of SEM ranged from 0.5 to 100 μg/L, the correlation coefficient was between 0.999 6 and 0.999 9. And the detection limit was 0.2 μg/kg. In addition, the relative standard deviation was 3.06%-6.56% and the standard recovery was 91.4%-103.6% respectively. Moreover, this method was further used to determine the contents of furacillin metabolites in three kinds of farmed shrimp (Penaeus monodon, Litopenaeus Vannamei and Macrobrachium rosenbergii). This method has the advantages of low detection limit, short detection time, good precision and accuracy, and can be used for the detection of SEM in farmed shrimp.

Key words： farmed shrimp; nitrofurazone; semicarbazide; microwave-assisted derivatization; ultra-performance liquid chromatography-tandem mass spectrometry

参考文献

[1] 程波, 舒秀君, 宋蓓, 等.甲壳类水产品氨基脲残留来源研究进展[J].广东海洋大学学报, 2018, 38(5):93-98.
CHENG B, SHU X J, SONG B, et al.Research progress of semicarbazide residues in crustacean aquatic products[J].Journal of Guangdong Ocean University, 2018, 38(5):93-98.
[2] 范清涛, 陈胜军, 邓建朝, 等.甲壳类水产品中氨基脲产生及控制方法研究进展[J].食品安全质量检测学报, 2020, 11(5):1 439-1 445.
FAN Q T, CHEN S J, DENG J C, et al.Research progress on the production and control method of semicarbazide in crustacean aquatic products[J].Journal of Food Safety & Quality Inspection, 2020, 11(5):1 439-1 445.
[3] 曹爱玲, 余招锋, 陈怡琳, 等.动物源食品中呋喃西林及其代谢物氨基脲研究进展[J].中国动物检疫, 2019, 36(6):62-67.
CAO A L, YU Z F, CHEN Y L, et al.Research progress of furacillin and its metabolite in food of animal origin[J].China Animal Quarantine, 2019, 36(6):62-67.
[4] WICKRAMANAYAKE P U, TRAN T C, HUGHES J G, et al.Simultaneous separation of nitrofuran antibiotics and their metabolites by using micellar electrokinetic capillary chromatography[J].Electrophoresis, 2006, 27(20):4 069-4 077.
[5] 吴烁, 张彪, 张万利, 等.荧光微球免疫层析方法定量检测水产品中四种硝基呋喃代谢物[J/OL].食品科学,2020.https://kns.cnki.net/kcms/detail/11.2206.TS.20201228.1609.026.html.
WU S, ZHANG B, ZHANG W L, et al.Quantitative determination of four nitrofuran metabolites in aquatic products by fluorescence microsphere immunochromatography[J/OL].Food Science,2020.https://kns.cnki.net/kcms/detail/11.2206.TS.20201228.1609.026.html.
[6] VASS M, DIBLIKOVA I, CERNOCH I, et al.ELISA for semicarbazide and its application for screening in food contamination[J].Analytica Chimica Acta, 2008, 608(1):86-94.
[7] O′MAHONY J, MOLONEY M, MCCONNELL R I, et al.Simultaneous detection of four nitrofuran metabolites in honey using amultiplexing biochip screening assay[J].Biosensors & Bioelectronics, 2011, 26(10):4 076-4 081.
[8] 魏涯, 岑剑伟, 郝淑贤, 等.高效液相色谱法测定池塘底泥中呋喃西林的研究[J].南方水产科学, 2014, 10(1):71-77.
WEI Y, CEN J W, HAO S X, et al.HPLC determination of nitrofurazone in sediment of aquacutue pond[J].Journal of Southern Fisheries Science, 2014, 10(1):71-77.
[9] TANG T, WEI F D,WANG X, et al.Determination of semicarbazide in fish by molecularly imprinted stir bar sorptive extraction coupled with high performance liquid chromatography[J].Journal of Chromatography B, 2018, 1 076:8-14.
[10] 中华人民共和国农业部. 农业部783号公告-1—2006 水产品中硝基呋喃类代谢物残留量的测定液相色谱-串联质谱法[S].北京:中国标准出版社,2006.
Ministry of Agriculture of the People′s Republic of China.Announcement No.783 of the Ministry of Agriculture-1—2006 Determination of nitrofuran metabolite residues in aquatic products by liquid chromatography-tandem mass spectrometry[S].Beijing:China Standard Press,2006.
[11] KAUFMANN A, BUTCHER P, MADEN K, et al.Determination of nitrofuran and chloramphenicol residues by high resolution mass spectrometry versus tandem quadrupole mass spectrometry[J].Analytica Chimica Acta, 2015, 862:41-52.
[12] ALDEEK F, HSIEH K C, UGOCHUKWU O N, et al.Accurate quantitation and analysis of nitrofuran metabolites, chloramphenicol, and florfenicol in seafood by ultrahigh-performance liquid chromatography-tandem mass spectrometry:Method validation and regulatory samples[J].Journal of Agricultural and Food Chemistry, 2018, 66(20):5 018-5 030.
[13] VALERA-TARIFA N M, PLAZA-BOLAÑOS P, ROMERO-GONZáLEA R, et al.Determination of nitrofuran metabolites in seafood by ultra high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry[J].Journal of Food Composition and Analysis, 2013, 30(2), 86-93.
[14] KIM D, KIM B, HYUNG S W, et al.An optimized method for the accurate determination of nitrofurans in chicken meat using isotope dilution-liquid chromatography/mass spectrometry[J].Journal of Food Composition and Analysis, 2015, 40:24-31.
[15] BARTOSZ S, ANDRZEJ P, MARTA G, et al.New method of analysis of nitrofurans and nitrofuran metabolites in different biological matrices using UHPLC-MS/MS[J].Journal of Veterinary Research, 2018, 62(2):161-166.
[16] 李攻科, 杜甫佑, 肖小华.微波辅助萃取技术在中药现代化中的应用[J].精细化工, 2007, 24(12):1 184-1 191.
LI G K, DU F Y, XIAO X H.Application of microwave-assisted extraction in the modernization of chinese traditional medicine[J].Fine Chemicals, 2007, 24(12):1 184-1 191.
[17] 尹怡, 张宏峰, 刘书贵, 等.微波辅助衍生-液相色谱-串联质谱法快速测定养殖水体中5种硝基呋喃类代谢物残留[J].质谱学报, 2016, 37(2):106-113.
YIN Y, ZHANG H F, LIU S G, et al.Determination of nitrofuran metabolites in fishery water by microwave assisted derivatization and liquid chromatography-tandem mass spectrometry[J].Journal of Chinese Mass Spectrometry Society, 2016, 37(2):106-113.
[18] LUO X Z, YU Y X, KONG X J, et al.Rapid microwave assisted derivatization of nitrofuran metabolites for analysis in shrimp by high performance liquid chromatography-fluorescence detector[J].Microchemical Journal, 2019, 150: 104189.
[19] 曹爱玲, 陈怡琳, 蔡路昀, 等.不同烘干温度对甲壳类水产品中氨基脲检出量的影响[J].中国动物检疫, 2020, 37(1):94-99.
CAO A L, CHEN Y L, CAI L Y, et al.The effects of different drying temperatures on the detectable amount of semicarbazide in crustacean aquatic products[J].China Animal Health Inspection, 2020, 37(1):94-99.
[20] 李剑, 陈泽暖, 蔡楠.超高效液相色谱-串联质谱法快速检测水产品中硝基呋喃类代谢物残留研究[J].江苏调味副食品, 2019, 36(1):34-37;44.
LI J, CHEN Z N, CAI N.Ultra high performance liquid chromatography-rapid determination of nitrofuran metabolites in aquatic products by tandem mass spectrometry[J].Jiangsu Condiment and Subsidiary Food, 2019, 36(1):34-37;44.
Options
文章导航

/

〈 〉

技术支持：北京玛格泰克科技发展有限公司