高效液相色谱法测定渔业用水中喹乙醇代谢物残留量
|
摘要
建立了固相萃取-高效液相色谱测定渔业用水中喹乙醇代谢物残留量的方法。3-甲基喹噁啉-2羧酸(MQCA)经PAX固相萃取柱纯化和富集,用含2%甲酸的乙酸乙酯溶液洗脱,甲醇和1. 0%甲酸水溶液作为流动相,经C18柱分离,10 min内出峰。MQCA在0. 01～1. 00 mg/m L范围内线性良好,相关系数为0. 999 91,外标法定量,MQCA的检出限为0. 01 mg/L,定量限为0. 02 mg/L,平均加标回收率为79. 0%～99. 3%,相对标准偏差(RSD)为7. 38%～9. 12%。利用该方法对山东省济宁市采煤塌陷区重点养殖区的渔业用水进行分析,8个站位中MQCA组分的含量均低于检出限。本方法适用于检测渔业用水中MQCA的残留,可为渔业环境保护提供技术支持。
A method of high performance liquid chromatography with solid phase extraction,purification and enrichment,followed with eluting with ethyl acetate containing 2% formic acid was established for detection of MQCA in fishery water. The samples were separated by the PAX C18 column with a mobile phase of methanol and 1. 0 % formic acid within 10 minutes. The linearity of MQCA over the concentration range 0. 01-1. 00 mg/m L was well by the external standard method,and the correlation coefficient was 0. 999 91. The detection limit of MQCA was 0. 01 mg/L based on the ratio of signal to noise( S/N = 3),and the quantitation limit of MQCA was 0. 02 mg/L based on the ratio of signal to noise( S/N = 10). The mean recoveries rate ranged from 79. 0% to 99. 3%,with relative standard deviation in the region of 7. 38%-9. 12%. The method was used to analyze fishery water from the important aquaculture areas in coal mining subsidence district. Each content of MQCA in the water samples from 8 stations was lower than the detection limit. In conclusion,this method is suitable for the detection of MQCA residues in fishery water,providing technological support for protecting fishery environment.
A method of high performance liquid chromatography with solid phase extraction,purification and enrichment,followed with eluting with ethyl acetate containing 2% formic acid was established for detection of MQCA in fishery water. The samples were separated by the PAX C18 column with a mobile phase of methanol and 1. 0 % formic acid within 10 minutes. The linearity of MQCA over the concentration range 0. 01-1. 00 mg/m L was well by the external standard method,and the correlation coefficient was 0. 999 91. The detection limit of MQCA was 0. 01 mg/L based on the ratio of signal to noise( S/N = 3),and the quantitation limit of MQCA was 0. 02 mg/L based on the ratio of signal to noise( S/N = 10). The mean recoveries rate ranged from 79. 0% to 99. 3%,with relative standard deviation in the region of 7. 38%-9. 12%. The method was used to analyze fishery water from the important aquaculture areas in coal mining subsidence district. Each content of MQCA in the water samples from 8 stations was lower than the detection limit. In conclusion,this method is suitable for the detection of MQCA residues in fishery water,providing technological support for protecting fishery environment.
引文
[1]陈杖榴.兽医药理学[M].北京:中国农业出版社,2002:240.
[2]潘葳,罗钦,刘文静,等.水产品与水产饲料中药物残留问题的分析及对策[J].福建农业学报,2011,26(6):1096-1100.
[3] Hutchinson M J,Young P B,Kennedy D G. Confirmation of carbadox and olaquindox metabolites in porcine liver using liquid chromatography-electrospray,tandem mass spectrometry[J]. J Chromatogr B,2005,816:15-20.
[4]杨祖英.食品检验[M].第二版.北京:化学工业出版社,2001:1-9.
[5]蒲红宇,胡兆群,李金明.论喹乙醇在水产饲料中的应用及安全性研究问题[J].水产养殖,2003,24(4):40-42.
[6]殷居易,倪梅林,寿成杰.鸡肉中喹乙醇、卡巴多及其代谢物的残留检测[J].中国兽药杂志,2006,40(1):11-15.
[7] Commission Regulation(EC)No. 2788/98. Amending Council Directive 70/524/EEC conceming additives in feedingstuffs as regards the withdrawal of authorisation for certain growth promoters[M]. Brussel:Eurropean Commission,1988.
[8]李燕,王小寒,马跃岗,等. HPLC测定水产品中喹乙醇代谢物残留量的方法探讨[J].南方农业,2014,8(34):55-58.
[9]刁晓平,孙根均,沈建忠.兽药的生态毒性及其对环境影响的研究进展[J].应用生态学报,2004,15(2):321-325.
[10]李道稳,邬良贤,李斌,等.喹乙醇残留检测研究进展[J].中国饲料,2016(22):25-28.
[11]梅光明,郑斌,陈雪昌,等.超高效液相色谱-质谱联用法测定水产品中喹乙醇代谢物残留量[J].浙江海洋学院学报(自然科学版),2010,29(3):254-259.
[12]贝亦江,王扬,何丰,等.高效液相色谱法测定水产品中喹乙醇代谢物残留量[J].食品科学,2013,34(1):255-288.
[13]赵东豪,黎智广,杨金兰,等.高效液相色谱-串联质谱测定水产品中残留的喹乙醇代谢物[J].分析实验室,2010,29(9):19-22.
[14]余海霞,张小军,杨会成,等.碱水解-高效液相色谱法测定草鱼组织中喹乙醇代谢的残留[J].中国渔业质量与标准,2012,1(2):67-70.
[15]薛良辰,彭玉芬,刘陆,等.超高效液相色谱-串联质谱法快速检测水产品中喹乙醇及其代谢物3-甲基-喹噁啉-2-羧酸的残留[J].现代食品科技,2013,29(2):413-415.
[16] Yamagata M,Low L K. Automated and ultrasensitive detection of methyl-3-quinoxaline-2-carboxylic acid by using gold nanoparticles probes SIA-rt-PCR[J]. Biosens Bioelectron,2009,24(9):2858-2863.
[17] Yao Y S,Shen J Z,Wu C M. Determinstion of 3-methyl quinoxaline-2-carboxylic acid porcine liver by high performance liquid chromatography[J]. China Anim Husb Vet Med,2011,38(2):187-190.
[18]欧阳姗,庞国芳,谢丽琪,等.动物组织中卡巴氧和喹乙醇以及相关代谢产物的液相色谱-串联质谱检测方法[J].分析测试学报,2008,27(6):590-594.
[19]肖利龙,花锦.超高效液相色谱法-串联质谱法测定兔肉中喹乙醇代谢物残留量[J].农产品加工,2015(12)53-55.
[20]林黎,谢丽琪,欧阳珊,等.液相色谱-串联质谱法测定牛奶和奶粉中卡巴氧和喹乙醇代谢物的残留量[J].分析实验室,2010,29(2):38-40.
[21]张冲.氟苯尼考、喹乙醇的环境行为及污染控制技术研究[D].南京:南京农业大学,2010.
[22]王林,丁焕中,钟家林,等. HPLC检测猪血浆和尿液中的喹烯酮及其主要代谢物[J].中国畜牧兽医,2011,38(12):52-56.
[23]李燕,王小寒,马跃岗,等. HPLC测定水产品中喹乙醇代谢物残留量的方法探讨[J].南方农业,2014,8(34):55-58.
[2]潘葳,罗钦,刘文静,等.水产品与水产饲料中药物残留问题的分析及对策[J].福建农业学报,2011,26(6):1096-1100.
[3] Hutchinson M J,Young P B,Kennedy D G. Confirmation of carbadox and olaquindox metabolites in porcine liver using liquid chromatography-electrospray,tandem mass spectrometry[J]. J Chromatogr B,2005,816:15-20.
[4]杨祖英.食品检验[M].第二版.北京:化学工业出版社,2001:1-9.
[5]蒲红宇,胡兆群,李金明.论喹乙醇在水产饲料中的应用及安全性研究问题[J].水产养殖,2003,24(4):40-42.
[6]殷居易,倪梅林,寿成杰.鸡肉中喹乙醇、卡巴多及其代谢物的残留检测[J].中国兽药杂志,2006,40(1):11-15.
[7] Commission Regulation(EC)No. 2788/98. Amending Council Directive 70/524/EEC conceming additives in feedingstuffs as regards the withdrawal of authorisation for certain growth promoters[M]. Brussel:Eurropean Commission,1988.
[8]李燕,王小寒,马跃岗,等. HPLC测定水产品中喹乙醇代谢物残留量的方法探讨[J].南方农业,2014,8(34):55-58.
[9]刁晓平,孙根均,沈建忠.兽药的生态毒性及其对环境影响的研究进展[J].应用生态学报,2004,15(2):321-325.
[10]李道稳,邬良贤,李斌,等.喹乙醇残留检测研究进展[J].中国饲料,2016(22):25-28.
[11]梅光明,郑斌,陈雪昌,等.超高效液相色谱-质谱联用法测定水产品中喹乙醇代谢物残留量[J].浙江海洋学院学报(自然科学版),2010,29(3):254-259.
[12]贝亦江,王扬,何丰,等.高效液相色谱法测定水产品中喹乙醇代谢物残留量[J].食品科学,2013,34(1):255-288.
[13]赵东豪,黎智广,杨金兰,等.高效液相色谱-串联质谱测定水产品中残留的喹乙醇代谢物[J].分析实验室,2010,29(9):19-22.
[14]余海霞,张小军,杨会成,等.碱水解-高效液相色谱法测定草鱼组织中喹乙醇代谢的残留[J].中国渔业质量与标准,2012,1(2):67-70.
[15]薛良辰,彭玉芬,刘陆,等.超高效液相色谱-串联质谱法快速检测水产品中喹乙醇及其代谢物3-甲基-喹噁啉-2-羧酸的残留[J].现代食品科技,2013,29(2):413-415.
[16] Yamagata M,Low L K. Automated and ultrasensitive detection of methyl-3-quinoxaline-2-carboxylic acid by using gold nanoparticles probes SIA-rt-PCR[J]. Biosens Bioelectron,2009,24(9):2858-2863.
[17] Yao Y S,Shen J Z,Wu C M. Determinstion of 3-methyl quinoxaline-2-carboxylic acid porcine liver by high performance liquid chromatography[J]. China Anim Husb Vet Med,2011,38(2):187-190.
[18]欧阳姗,庞国芳,谢丽琪,等.动物组织中卡巴氧和喹乙醇以及相关代谢产物的液相色谱-串联质谱检测方法[J].分析测试学报,2008,27(6):590-594.
[19]肖利龙,花锦.超高效液相色谱法-串联质谱法测定兔肉中喹乙醇代谢物残留量[J].农产品加工,2015(12)53-55.
[20]林黎,谢丽琪,欧阳珊,等.液相色谱-串联质谱法测定牛奶和奶粉中卡巴氧和喹乙醇代谢物的残留量[J].分析实验室,2010,29(2):38-40.
[21]张冲.氟苯尼考、喹乙醇的环境行为及污染控制技术研究[D].南京:南京农业大学,2010.
[22]王林,丁焕中,钟家林,等. HPLC检测猪血浆和尿液中的喹烯酮及其主要代谢物[J].中国畜牧兽医,2011,38(12):52-56.
[23]李燕,王小寒,马跃岗,等. HPLC测定水产品中喹乙醇代谢物残留量的方法探讨[J].南方农业,2014,8(34):55-58.