动物源性食品中硝基呋喃代谢物的超高效液相色谱-串联质谱测定法
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摘要
目的建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定8种基质(鸡肉、鸭肉、牛肉、猪肉、鱼肉、虾肉、海参、鸡肝)中呋喃它酮、呋喃西林、呋喃妥因和呋喃唑酮4种硝基呋喃代谢物的检测方法。方法试样经2-硝基苯甲醛衍生化,调节pH值至7.2～7.6,经Oasis HLB固相萃取柱净化,由乙酸乙酯洗脱,流动相定容,采用选择反应监测(SRM)模式检测,电喷雾正离子(ESI+)模式电离,同位素内标法定量。结果硝基呋喃代谢物在0.5～30.0μg/L范围内线性关系良好(r>0.99)。方法的最低检出限为0.5μg/kg,在0.5、1.0、2.0μg/kg的3个添加水平的回收率为60.9%～103.5%,相对标准偏差(RSD,n=6)在2.1%～11.1%之间。结论超高效液相色谱-串联质谱测定法快速、灵敏、准确,适合动物源性食品中硝基呋喃代谢物的测定。
Objective To establish a method for the determination of nitrofuran metabolites(furantazone,furacilin,furantoin and furazolidone) in eight animal derived matrices(including chicken muscle,duck muscle,beef muscle,pork muscle,fish muscle,prawn muscle,sea cucumber,chicken liver) by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods Samples were derivatized with 2-nitrobenzaldehyde and adjusted the pH value to 7.2-7.6. The derivatized solutions were cleaned up by Oasis HLB solid extraction column(SPE)and the target compounds were eluted with ethylacetate.The analysis were carried out on electrospray ion( ESI +) source in the positive mode and monitored by selective reaction monitoring(SRM) mode. The internal standard isotope dilution method was used for quantification. Results The calibration curve showed a good linearity in the range of 0.5-30.0 μg/L and the correlation coefficient(r) was higher than 0.99. The limit of determinations was 0.5 μg/kg. At the spiked levels of 0.5,1.0 and 2.0 μg/kg,the recoveries of nitrofuran metabolites ranged from 60.9% to 103.5% and the relative standard deviation(RSD,n=6) ranged from 2.1% to 11.1%. Conclusion The method of UPLC-MS/MS is simple,rapid,sensitive and suitable for the qualitative and quantitative analysis of nitrofuran metabolites in animal derived food.
Objective To establish a method for the determination of nitrofuran metabolites(furantazone,furacilin,furantoin and furazolidone) in eight animal derived matrices(including chicken muscle,duck muscle,beef muscle,pork muscle,fish muscle,prawn muscle,sea cucumber,chicken liver) by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods Samples were derivatized with 2-nitrobenzaldehyde and adjusted the pH value to 7.2-7.6. The derivatized solutions were cleaned up by Oasis HLB solid extraction column(SPE)and the target compounds were eluted with ethylacetate.The analysis were carried out on electrospray ion( ESI +) source in the positive mode and monitored by selective reaction monitoring(SRM) mode. The internal standard isotope dilution method was used for quantification. Results The calibration curve showed a good linearity in the range of 0.5-30.0 μg/L and the correlation coefficient(r) was higher than 0.99. The limit of determinations was 0.5 μg/kg. At the spiked levels of 0.5,1.0 and 2.0 μg/kg,the recoveries of nitrofuran metabolites ranged from 60.9% to 103.5% and the relative standard deviation(RSD,n=6) ranged from 2.1% to 11.1%. Conclusion The method of UPLC-MS/MS is simple,rapid,sensitive and suitable for the qualitative and quantitative analysis of nitrofuran metabolites in animal derived food.
引文
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[2]王传现,黄帆,王敏,等.液相色谱-串联质谱联用法测定水产品中残留的硝基呋喃类药物的代谢物[J].色谱,2013,31(3):206-210.
[3]谢云峰,李少晖,任丹丹,等.超高效液相色谱-串联质谱法测定猪肉中硝基呋喃代谢物[J].分析测试技术与仪器,2015,21(4):212-217.
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[5]孙涛,胡开峰,乔昆云,等.超高效液相色谱-串联质谱法测定水产品中硝基呋喃代谢物残留[J].分析仪器,2010(5):27-31.
[6]刘辉,梁徳沛,花铁果,等.食品中硝基呋喃类药物及其代谢物残留技术的研究进展[J].食品安全与质量检测学报,2013,4(2):383-388.
[7]刘伯林,谢继安,赵紫微,等.超高效液相色谱-串联质谱法测定动物源性食品中硝基呋喃代谢物[J].食品安全与质量检测学报,2015,5(2):421-427.
[8]徐一平,金征宇,胥传来. ELISA方法检测呋喃妥因代谢物1-氨基乙内酰脲[J].食品工业科技,2008,29(8):272-275.
[9]中华人民共和国国家进出口商品检验局.SN 0530-1996出口肉中呋喃唑酮残留量的检验方法液相色谱法[S/OL].(1996-10-01)[2017-10-15].http://down.foodmate.net/standard/sort/4/1704.html.
[10]葛宝坤,王云凤,常春艳,等.测定鸡肉、水产品中四种硝基呋喃类药物残留量的固相萃取-液相色谱法[J].分析测试学报,2003,22(5):91-93.
[11]林黎明,林回春,高彦宗,等.液相色谱/串联质谱线性组合法测定动物组织中硝基呋喃代谢产物[J].分析化学,2005,33(8):1081-1086.
[12]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.
[13]宋利军,于晖,程鑫,等.液相色谱-串联质谱法检测动物性食品中硝基呋喃代谢产物的残留[J].中国卫生检验杂志,2017,27(3):321-323.
[14]刘柏林,谢继安,单晓梅,等.超高压液相色谱-串联质谱法同时测定鸡蛋中4种硝基呋喃代谢物残留[J].中国食品卫生杂志,2014,26(5):469-473.
[15]高洁,朱莉萍,倪永付,等.超高效液相色谱-串联质谱法测定多脂肪类动物源性食品中硝基呋喃代谢物[J].食品安全质量检测学报,2018,9(6):1362-1368.
[16]高月明,冯笑军,李倩莹.超高效液相色谱-串联质谱法测定淡水鱼中硝基呋喃类代谢物残留[J].食品安全质量检测学报,2017,8(8):3231-3236.
[17]林涛,樊建麟,杨东顺,等.液液萃取柱-液相色谱-串联质谱法测定乳制品中硝基呋喃类代谢物残留[J].分析试验室,2015,34(11):1281-1285.
[18]王跃,尹燕杰,赵丹,等.超高效液相色谱-串联质谱法测定水产品中的硝基呋喃代谢物[J].化学分析计量,2018,27(5):43-47.
[19]雷美康,彭芳,祝子铜,等.高效液相色谱-串联质谱法测定蜂蜡中硝基呋喃类代谢物[J].分析试验室,2015,34(10):1174-1177.
[20]庞国芳,张进杰,曹彦忠,等.高效液相色谱-串联质谱法测定家禽组织中硝基呋喃类抗生素代谢物残留的研究[J].食品科学,2005,26(10):160-165.
[21]彭涛,邱月明,李淑娟,等.高效液相色谱-串联质谱法测定动物肌肉中硝基呋喃类抗生素代谢物[J].检验检疫科学,2003,13(6):23-26.
[2]王传现,黄帆,王敏,等.液相色谱-串联质谱联用法测定水产品中残留的硝基呋喃类药物的代谢物[J].色谱,2013,31(3):206-210.
[3]谢云峰,李少晖,任丹丹,等.超高效液相色谱-串联质谱法测定猪肉中硝基呋喃代谢物[J].分析测试技术与仪器,2015,21(4):212-217.
[4]田蕴,罗晓琴.水产品硝基呋喃类药物残留检测[J].动物保健,2006(7):45-47.
[5]孙涛,胡开峰,乔昆云,等.超高效液相色谱-串联质谱法测定水产品中硝基呋喃代谢物残留[J].分析仪器,2010(5):27-31.
[6]刘辉,梁徳沛,花铁果,等.食品中硝基呋喃类药物及其代谢物残留技术的研究进展[J].食品安全与质量检测学报,2013,4(2):383-388.
[7]刘伯林,谢继安,赵紫微,等.超高效液相色谱-串联质谱法测定动物源性食品中硝基呋喃代谢物[J].食品安全与质量检测学报,2015,5(2):421-427.
[8]徐一平,金征宇,胥传来. ELISA方法检测呋喃妥因代谢物1-氨基乙内酰脲[J].食品工业科技,2008,29(8):272-275.
[9]中华人民共和国国家进出口商品检验局.SN 0530-1996出口肉中呋喃唑酮残留量的检验方法液相色谱法[S/OL].(1996-10-01)[2017-10-15].http://down.foodmate.net/standard/sort/4/1704.html.
[10]葛宝坤,王云凤,常春艳,等.测定鸡肉、水产品中四种硝基呋喃类药物残留量的固相萃取-液相色谱法[J].分析测试学报,2003,22(5):91-93.
[11]林黎明,林回春,高彦宗,等.液相色谱/串联质谱线性组合法测定动物组织中硝基呋喃代谢产物[J].分析化学,2005,33(8):1081-1086.
[12]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.
[13]宋利军,于晖,程鑫,等.液相色谱-串联质谱法检测动物性食品中硝基呋喃代谢产物的残留[J].中国卫生检验杂志,2017,27(3):321-323.
[14]刘柏林,谢继安,单晓梅,等.超高压液相色谱-串联质谱法同时测定鸡蛋中4种硝基呋喃代谢物残留[J].中国食品卫生杂志,2014,26(5):469-473.
[15]高洁,朱莉萍,倪永付,等.超高效液相色谱-串联质谱法测定多脂肪类动物源性食品中硝基呋喃代谢物[J].食品安全质量检测学报,2018,9(6):1362-1368.
[16]高月明,冯笑军,李倩莹.超高效液相色谱-串联质谱法测定淡水鱼中硝基呋喃类代谢物残留[J].食品安全质量检测学报,2017,8(8):3231-3236.
[17]林涛,樊建麟,杨东顺,等.液液萃取柱-液相色谱-串联质谱法测定乳制品中硝基呋喃类代谢物残留[J].分析试验室,2015,34(11):1281-1285.
[18]王跃,尹燕杰,赵丹,等.超高效液相色谱-串联质谱法测定水产品中的硝基呋喃代谢物[J].化学分析计量,2018,27(5):43-47.
[19]雷美康,彭芳,祝子铜,等.高效液相色谱-串联质谱法测定蜂蜡中硝基呋喃类代谢物[J].分析试验室,2015,34(10):1174-1177.
[20]庞国芳,张进杰,曹彦忠,等.高效液相色谱-串联质谱法测定家禽组织中硝基呋喃类抗生素代谢物残留的研究[J].食品科学,2005,26(10):160-165.
[21]彭涛,邱月明,李淑娟,等.高效液相色谱-串联质谱法测定动物肌肉中硝基呋喃类抗生素代谢物[J].检验检疫科学,2003,13(6):23-26.