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
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摘要
以水产品中的硝基呋喃类代谢物残留为研究对象,建立超高效液相色谱-串联质谱(UPLC-MS/MS)测定水产品中硝基呋喃类代谢物残留分析方法。结果显示:硝基呋喃类代谢物在1. 0～100. 0 ng/mL的范围内线性关系良好,相对回收率为86. 2%～108%,相对标准偏差为3. 4%～9. 6%,检出限为0. 25μg/kg,定量限为0. 5μg/kg。与以往采用的超高效液相色谱-串联质谱方法相比,新建方法操作简单、快速、准确,是定量检测水产品中硝基呋喃类代谢物残留的有效技术手段。
Based on the residue of nitrofuran metabolites in aquatic products,a super high performance liquid chromatography-tandem mass spectrometry(uplc-ms/MS) was established to determine the residue of nitrofurans metabolites in aquatic products. The results were good in the range of 1 ～ 100. 0 ng/mL,and the relative recovery rate was 86. 2 ～ 108%,the relative standard deviation was 3. 4 ～ 9. 6%,and the detection limit was 0. 25 μg/kg,and the quantitative limit was 0. 5 μg/kg. Compared with the ultra high performance liquid chromatography-tandem mass spectrometry method,the new method is simple,rapid and accurate,which provides effective and practical technical means for quantitative detection of nitrofuran metabolites in aquatic products.
Based on the residue of nitrofuran metabolites in aquatic products,a super high performance liquid chromatography-tandem mass spectrometry(uplc-ms/MS) was established to determine the residue of nitrofurans metabolites in aquatic products. The results were good in the range of 1 ～ 100. 0 ng/mL,and the relative recovery rate was 86. 2 ～ 108%,the relative standard deviation was 3. 4 ～ 9. 6%,and the detection limit was 0. 25 μg/kg,and the quantitative limit was 0. 5 μg/kg. Compared with the ultra high performance liquid chromatography-tandem mass spectrometry method,the new method is simple,rapid and accurate,which provides effective and practical technical means for quantitative detection of nitrofuran metabolites in aquatic products.
引文
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[8]魏涯,岑建伟,郝淑贤,等.高效液相色谱法测定泥潭底泥中呋喃西林的研究[J].水产科学,2014(1):71-77.
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[10]柳爱春,刘超,赵芸,等.免疫胶体金法快速检测水产品中硝基呋喃类代谢物的研究[J].浙江农业学报,2013(1):95-102.
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[12]张敏,桑丽雅,王振国,等.用于水产品中硝基呋喃类代谢物检测的胶体金快速检测试剂板的研制[J].中国食品卫生杂志,2013(1):32-36.
[13]DU N N,CHEN M M,SHENG L Q,et al.Determination of nitrofuran metabolites in shrimp by high performance liquid chromatography with fluorescence detection and liquid chrome to graphytandem mass spectrometry using a new derivatization reagent[J].Journal of chromatography A,2014(1):90-96.
[14]SHENG L Q,CHEN M M,CHEN S S,et al.High-performance liquid chromatography with fluorescence detection for the determination of nitrofuran metabolites in pork muscle[J].Food additives and contaminants,2013(12):2114-2122.
[15]AN H,HENRY M,CAIN T,et al.Determination of total nitrofuran metabolites in shrimp muscle using liquid chromatography tandem mass spectrometry in the atmospheric pressure chemical ionization mode[J].Journal of AOACinternational,2012(4):1222-1233.
[16]RODZIEWICZ L,ZAWADZKA I.Development and validation of a new method for determining nitrofuran metabolites in bovine urine using liquid chromatography-tandem mass spectrometry[J].Roczniki panstwowego zakladu higieny,2013(4):285-291.
[2]见明,章元琅,颜闵,等.硝基呋喃类代谢物的结构修饰[J].医药工业,1987(7):330.
[3]HOOGENBOOM L A,VAN BRUCHEM G D,SONNE K,et al.Absorption of a mutagenic metabolite released from protein-bound residues of furazolidone[J].Eniviron toxicol pharmacol,2002(3/4):273-287.
[4]MCCALLA D R.Mutagenicity of nitrofuran derivatives:review[J].Environ Mutagen,1983(5):745-765.
[5]MCCRACKEN R J,KENNEDY D G.Determination of the furazolidone metabolite,3-amino-2-oxazolidinone,in porcine tissues using liquid chromatography thermospray mass spectrometry and the occurrence of residues in pigs prduced in Northern Ireland[J].Journal of chromatography B,1997(1):87-94.
[6]谭志军,崔敏秀,冷凯良,等.呋喃西林和呋喃唑酮代谢物在大鳞鲆组织中的消除规律[J].中山大学学报(自然科学版),2008(S1):63-68.
[7]赵东豪,黎智广,李刘冬,等.虾苗使用呋喃西林和呋喃唑酮的残留评估[J].水产科学,2012(3):54-58.
[8]魏涯,岑建伟,郝淑贤,等.高效液相色谱法测定泥潭底泥中呋喃西林的研究[J].水产科学,2014(1):71-77.
[9]中华人民共和国农业部.中华人民共和国农业部公告第235号[J].兽药杂志,2003(2/3/4):19.
[10]柳爱春,刘超,赵芸,等.免疫胶体金法快速检测水产品中硝基呋喃类代谢物的研究[J].浙江农业学报,2013(1):95-102.
[11]LEITNER A,ZOLLNER P,LINDNER W.Determination of the metabolites of nitrofuran antibiotics in animal tissue by highperformance liquid chromatography-tandem mass spectrometry[J].Chromatogr A,2001(1/2):49-58.
[12]张敏,桑丽雅,王振国,等.用于水产品中硝基呋喃类代谢物检测的胶体金快速检测试剂板的研制[J].中国食品卫生杂志,2013(1):32-36.
[13]DU N N,CHEN M M,SHENG L Q,et al.Determination of nitrofuran metabolites in shrimp by high performance liquid chromatography with fluorescence detection and liquid chrome to graphytandem mass spectrometry using a new derivatization reagent[J].Journal of chromatography A,2014(1):90-96.
[14]SHENG L Q,CHEN M M,CHEN S S,et al.High-performance liquid chromatography with fluorescence detection for the determination of nitrofuran metabolites in pork muscle[J].Food additives and contaminants,2013(12):2114-2122.
[15]AN H,HENRY M,CAIN T,et al.Determination of total nitrofuran metabolites in shrimp muscle using liquid chromatography tandem mass spectrometry in the atmospheric pressure chemical ionization mode[J].Journal of AOACinternational,2012(4):1222-1233.
[16]RODZIEWICZ L,ZAWADZKA I.Development and validation of a new method for determining nitrofuran metabolites in bovine urine using liquid chromatography-tandem mass spectrometry[J].Roczniki panstwowego zakladu higieny,2013(4):285-291.