高效液相色谱-串联质谱法测定水产品中喹乙醇残留量
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摘要
目的建立高效液相色谱-串联质谱联用法测定水产品中喹乙醇残留量的方法。方法以罗非鱼为实验样品,样品经乙腈提取、正己烷脱脂,以乙腈-0.5 mmol乙酸铵甲酸溶液(10:90, V:V)为流动相进行等度洗脱、色谱柱Poroshell 120 EC-C_(18)(50mm×2.1mm, 2.7μm)分离,在多反应监测(multiple reactionmonitoring, MRM)模式下进行三重四极杆质谱检测。结果喹乙醇在0.02～0.4 mg/kg范围内线性兲系良好,检出限为0.4μg/kg,加标回收率(n=6)为93.8%～97.0%,相对标准偏差为2.10%～8.02%。结论该方法简单、快速、灵敏度高、准确可靠,可用于批量水产品样品喹乙醇残留量的测定。
Objective To establish a method for the determination of olaquindox residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). Methods Tilapia samples were extracted by acetonitrile, and purified by hexane. The obtained target compound were separated by high performance liquid chromatography using Poroshell 120 EC-C_(18)(50 mm× 2.1 mm, 2.7 μm) column with isocratic elution of acetonitrile-0.5 mmol ammonium acetate formic acid solution(10:90, V:V), and were detected by HPLC-MS/MS with multiple reaction monitoring(MRM) mode. Results Olaquindox had good linearity in the range of 0.02-0.4 mg/L. The limit of detection was 0.4 mg/kg, and the standard recovery rates were 93.8%-97.0%(n=6), with the relative standard deviation of 2.10%-8.02%. Conclusion This method is simple, rapid, sensitive, accurate and reliable, which can be used for the determination of residual amount of olaquindox in batches of aquatic products.
Objective To establish a method for the determination of olaquindox residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). Methods Tilapia samples were extracted by acetonitrile, and purified by hexane. The obtained target compound were separated by high performance liquid chromatography using Poroshell 120 EC-C_(18)(50 mm× 2.1 mm, 2.7 μm) column with isocratic elution of acetonitrile-0.5 mmol ammonium acetate formic acid solution(10:90, V:V), and were detected by HPLC-MS/MS with multiple reaction monitoring(MRM) mode. Results Olaquindox had good linearity in the range of 0.02-0.4 mg/L. The limit of detection was 0.4 mg/kg, and the standard recovery rates were 93.8%-97.0%(n=6), with the relative standard deviation of 2.10%-8.02%. Conclusion This method is simple, rapid, sensitive, accurate and reliable, which can be used for the determination of residual amount of olaquindox in batches of aquatic products.
引文
[1]王仁华,练小华,谢益根.饲料中喹乙醇的应用效果研究[J].饲料与畜牧,2017,(2):56-57.Wang RH,Lian XH,Xie YG.Research application effect of olaquindox in feed[J].Feed Husb,2017,(2):56-57.
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[3]邱建东,林世武.动物源性食品中喹乙醇的残留及危害[J].中国畜牧兽医文摘,2017,33(4):23Qiu JD,Lin SW.Residues and harms of olaquindox in animal-derived foods[J].Chin Abstract Anim Husb Vet Med,2017,33(4):23.
[4]SC/T 3019-2004水产品中喹乙醇残留量的测定液相色谱法[S].SC/T 3019-2004 Determination of olaquindox residues in fishery products-High-performance of liquid chromatography[S].
[5]刘淳.超高效液相色谱测定猪肉中喹乙醇的残留量[J].分析仪器,2017,(2):44-47.Liu C.Determination of olaquindox residues in Pork by ultraperformance liquid chromatography[J].Anal Instrum,2017,(2):44-47.
[6]于慧娟,毕士川,黄冬梅,等.高效液相色谱法测定水产品中喹乙醇的残留量[J].分析科学学报,2004,20(3):281-283.Yu HY,Bi SC,Huang DM,et al.Determination of olaquindox residues in fishery products high-performance of liquid chromatography[J].J Anal Sci,2004,20(3):281-283.
[7]韩梅,于盟盟,梁娟,等.高效液相色谱法测定水产品中喹乙醇影响因素及消除[J].河北渔业,2018,(3):48-50.Han M,Yu MM,Liang J,et al.Determination of the factors affecting olaquindox in fishery products by high performance liquid chromatography[J].Hebei Fish,2018,(3):48-50.
[8]郭霞,孙振中,戚隽渊,等.南美白对虾中喹乙醇及其代谢物3-甲基-喹恶啉-2-羧酸残留的高效液相色谱-串联质谱检测[J].中国农业大学学报,2014,19(1):156-160.Guo X,Sun Z,Qi JY,et al.Determination of residual olaquindox and methyl-3-quinoxaline-2-carboxylic acid in penaeusvannamei by HPLCMS/MS[J].J China Agric Univ,2014,19(1):156-160.
[9]耿宁,卢剑.高效液相色谱-串联质谱法测定肌肉组织中4种兽药残留[J].肉类研究,2017,31(8):39-43.Geng N,Lu J.Determination of four veterinary drug residues in muscle tissue by high performance liquid chromatography-tandem mass spectrometry[J].Meat Res,2017,31(8):39-43.
[10]陈俊秀,张秀清,李文廷,等.超高效液相色谱-串联质谱法测定奶酪中喹乙醇及其代谢物[J].食品安全质量检测学报,2018,9(12):3171-3176.Chen JX,Zhang XQ,Li WT,et al.Determination of olaquindox and its metabolite in cheese by ultra performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2018,9(12):3171-3176.
[11]欧阳姗,庞国芳,谢丼琪,等.动物组织中卡巴氧和喹乙醇以及相兲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.Ou YS,Pang GF,Xie LQ,et al.Determination of the residues of carbadox,olaquindox and related metabolites in bovine and porcine muscle and liver tissues by LC-MS/MS[J].J Instrum Anal,2008,27(6):590-594.
[12]裴星瑶,王旗,谢洁,等.荧光微球免疫层析法快速检测鸡饲料中喹乙醇的含量[J].中国兽医杂志,2016,52(9):83-85,90.Pei XY,Wang Q,Xie J,et al.Rapid detection of olaquindox in chicken feed by fluorescent microsphere immunochromatography[J].Chin J Vet Med,2016,52(9):83-85,90.
[13]郑玲,吴玉杰,赵永峰,等.高效液相色谱-串联质谱法测定动物源食品中喹乙醇与卡巴氧残留量[J].分析测试学报,2014,33(1):21-26.Zhen L,Wu YJ,Zhao YF,et al.Determination of olaquindox and caboxygen in animal foodstuffs byhigh performance liquid chromatographytandem mass spectrometry[J].J Instrum Anal,2014,33(1):21-26.
[14]曾静,朱宽正,王鹏,等.高效液相色谱-串联质谱法测定水产品中喹乙醇[J].中国食品卫生杂志,2006,18(5):423-425.Zeng J,Zhu KZ,Wang P,et al.Determination of olaquindox in fishery products High-performance of liquid chromatography-tandem mass spectrometry[J].Chin J Food Hyg,2006,18(5):423-425.
[15]张翠芬.同位素内标法测定动物源性食品中喹乙醇含量[J].中国食品添加剂分析测试,2017,(4):178-183.Zhang CF.Determination of olaquindox in animal-derived foods by isotope internal standard method[J].China Food Addit Anal Test,2017,(4):178-183.
[2]刘沫飞,徐世文,吴发关,等.雏鸡喹乙醇中毒血液生化指标测定[J].动物医学进展,2012,33(9):74-77.Liu MF,Xu SW,Wu FX,et al.Determination of blood biochemical indexes in chicken olaquindox poisoning[J].Prog Vet Med,2012,33(9):74-77.
[3]邱建东,林世武.动物源性食品中喹乙醇的残留及危害[J].中国畜牧兽医文摘,2017,33(4):23Qiu JD,Lin SW.Residues and harms of olaquindox in animal-derived foods[J].Chin Abstract Anim Husb Vet Med,2017,33(4):23.
[4]SC/T 3019-2004水产品中喹乙醇残留量的测定液相色谱法[S].SC/T 3019-2004 Determination of olaquindox residues in fishery products-High-performance of liquid chromatography[S].
[5]刘淳.超高效液相色谱测定猪肉中喹乙醇的残留量[J].分析仪器,2017,(2):44-47.Liu C.Determination of olaquindox residues in Pork by ultraperformance liquid chromatography[J].Anal Instrum,2017,(2):44-47.
[6]于慧娟,毕士川,黄冬梅,等.高效液相色谱法测定水产品中喹乙醇的残留量[J].分析科学学报,2004,20(3):281-283.Yu HY,Bi SC,Huang DM,et al.Determination of olaquindox residues in fishery products high-performance of liquid chromatography[J].J Anal Sci,2004,20(3):281-283.
[7]韩梅,于盟盟,梁娟,等.高效液相色谱法测定水产品中喹乙醇影响因素及消除[J].河北渔业,2018,(3):48-50.Han M,Yu MM,Liang J,et al.Determination of the factors affecting olaquindox in fishery products by high performance liquid chromatography[J].Hebei Fish,2018,(3):48-50.
[8]郭霞,孙振中,戚隽渊,等.南美白对虾中喹乙醇及其代谢物3-甲基-喹恶啉-2-羧酸残留的高效液相色谱-串联质谱检测[J].中国农业大学学报,2014,19(1):156-160.Guo X,Sun Z,Qi JY,et al.Determination of residual olaquindox and methyl-3-quinoxaline-2-carboxylic acid in penaeusvannamei by HPLCMS/MS[J].J China Agric Univ,2014,19(1):156-160.
[9]耿宁,卢剑.高效液相色谱-串联质谱法测定肌肉组织中4种兽药残留[J].肉类研究,2017,31(8):39-43.Geng N,Lu J.Determination of four veterinary drug residues in muscle tissue by high performance liquid chromatography-tandem mass spectrometry[J].Meat Res,2017,31(8):39-43.
[10]陈俊秀,张秀清,李文廷,等.超高效液相色谱-串联质谱法测定奶酪中喹乙醇及其代谢物[J].食品安全质量检测学报,2018,9(12):3171-3176.Chen JX,Zhang XQ,Li WT,et al.Determination of olaquindox and its metabolite in cheese by ultra performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2018,9(12):3171-3176.
[11]欧阳姗,庞国芳,谢丼琪,等.动物组织中卡巴氧和喹乙醇以及相兲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.Ou YS,Pang GF,Xie LQ,et al.Determination of the residues of carbadox,olaquindox and related metabolites in bovine and porcine muscle and liver tissues by LC-MS/MS[J].J Instrum Anal,2008,27(6):590-594.
[12]裴星瑶,王旗,谢洁,等.荧光微球免疫层析法快速检测鸡饲料中喹乙醇的含量[J].中国兽医杂志,2016,52(9):83-85,90.Pei XY,Wang Q,Xie J,et al.Rapid detection of olaquindox in chicken feed by fluorescent microsphere immunochromatography[J].Chin J Vet Med,2016,52(9):83-85,90.
[13]郑玲,吴玉杰,赵永峰,等.高效液相色谱-串联质谱法测定动物源食品中喹乙醇与卡巴氧残留量[J].分析测试学报,2014,33(1):21-26.Zhen L,Wu YJ,Zhao YF,et al.Determination of olaquindox and caboxygen in animal foodstuffs byhigh performance liquid chromatographytandem mass spectrometry[J].J Instrum Anal,2014,33(1):21-26.
[14]曾静,朱宽正,王鹏,等.高效液相色谱-串联质谱法测定水产品中喹乙醇[J].中国食品卫生杂志,2006,18(5):423-425.Zeng J,Zhu KZ,Wang P,et al.Determination of olaquindox in fishery products High-performance of liquid chromatography-tandem mass spectrometry[J].Chin J Food Hyg,2006,18(5):423-425.
[15]张翠芬.同位素内标法测定动物源性食品中喹乙醇含量[J].中国食品添加剂分析测试,2017,(4):178-183.Zhang CF.Determination of olaquindox in animal-derived foods by isotope internal standard method[J].China Food Addit Anal Test,2017,(4):178-183.