HPLC法测定蔬菜中3种喹诺酮类抗生素
|
摘要
建立蔬菜中3种喹诺酮类抗生素的HPLC分析方法,对蔬菜中喹诺酮类抗生素的残留情况进行评估。采用Hedera-C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.1%甲酸水溶液(20∶80,V/V)为流动相,流速1 m L/min,柱温25℃,检测波长280 nm,进样体积20μL。在15 min内3个被测组分完全分离,线性回归方程显示3种抗生素的峰面积与质量浓度呈现良好的线性关系。蔬菜中的诺氟沙星、环丙沙星、恩诺沙星的加样回收率(n=3)分别在92%～94%,相对标准偏差(RSD)小于3.0%。检测限为60～120 g/kg,定量限为180～360 g/kg。该方法适用于食用蔬菜样品的分析,但蔬菜中此类抗生素富集问题也急需引起广泛关注。
To establish a HPLC method for the determination of three quinolone antibiotics in vegetables,and to evaluate the residues of quinolones in vegetables. Hedera-C18 column(250 mm×4.6 mm,5 μm);acetonitrile-0.1% formic acid aqueous solution(20∶80,V/V) as mobile phase,flow rate 1 m L/min;column temperature 25 ℃,detection wavelength at 280 nm,the injection volume was 20 μL. The three tested components were completely separated within 15 min. The linear regression equation showed a good linear relationship between the peak area and concentration of the three antibiotics. The recoveries(n=3) of the three quinolone compounds in vegetables ranged 92%～94%,and the relative standard deviation(RSD) was less than 3.0%. The detection limit was 60～120 g/kg,the limit of quantification was 180～360 g/kg. This method can meet the analysis requirements of actual vegetable samples, and the problem of enrichment of quinolones in vegetables was urgently needed to attract widespread attention.
To establish a HPLC method for the determination of three quinolone antibiotics in vegetables,and to evaluate the residues of quinolones in vegetables. Hedera-C18 column(250 mm×4.6 mm,5 μm);acetonitrile-0.1% formic acid aqueous solution(20∶80,V/V) as mobile phase,flow rate 1 m L/min;column temperature 25 ℃,detection wavelength at 280 nm,the injection volume was 20 μL. The three tested components were completely separated within 15 min. The linear regression equation showed a good linear relationship between the peak area and concentration of the three antibiotics. The recoveries(n=3) of the three quinolone compounds in vegetables ranged 92%～94%,and the relative standard deviation(RSD) was less than 3.0%. The detection limit was 60～120 g/kg,the limit of quantification was 180～360 g/kg. This method can meet the analysis requirements of actual vegetable samples, and the problem of enrichment of quinolones in vegetables was urgently needed to attract widespread attention.
引文
[1]Kools S A E, Moltmann J F, Knacker T. Estimating the use of veterinary medicines in the European union[J].Regulatory Toxicology&Pharmacology, 2008, 50(1):59-65.
[2]Dosogne H,Meyer E,Sturk A,et al. Effect of enrofloxacin treatment on plasma endotoxin during bovine Escherichia colimastitis[J]. Inflammation Research, 2002, 51(4):201-205.
[3]Metcalfe C D,Miao X S,Koenig B G,et al. Distribution of acidic and neutral drugs in surface waters near sewage treatment plants in the lower Great Lakes, Canada[J].Environmental Toxicology and Chemistry,2003,22(12):2 881-2 890.
[4]Vieno N, Tuhkanen T, Kronberg L. Elimination of pharmaceuticals in sewage treatment plants in Finland[J].Water Research,2007,41(5):1 001-1 012.
[5]Aust M O,Godlinski F,Travis G R,et al. Distribution of sulfamethazine,chlortetracycline and tylosin in manure and soil of Canadian feedlots after subtherapeutic use in cattle[J]. Environmental Pollution,2008(3):1 240-1251.
[6]Karci A, Balcioglu I A. Investigation of the tetracycline,sulfonamide,and fluoroquinolone antimicrobial compounds in animal manure and agricultural soils in Turkey[J].Science of the Total Environment,2009(16):4 652-4 664.
[7]张慧敏,章明奎,顾国平.浙北地区畜禽粪便和农田土壤中四环素类抗生素残留[J].生态与农村环境学报,2008(3):69-73.
[8]潘杰平.浅谈兽药残留对食品安全的影响[J].中国动物保健,2018,20(5):8-9.
[9]农业部畜牧兽医局.农业部发布动物性食品中兽药最高残留限量[J].中国兽药杂志,2003,25(2):5-11.
[10]刘佳佳,金芬,佘永新,等.液相色谱-串联质谱法测定牛奶中5种多肽类抗生素[J].分析化学,2011,39(5):652-657.
[11]Herreraherrera A V,Hernándezborges J,Rodríguezdelgado M A,et al. Determination of quinolone residues in infant and young children powdered milk combining solidphase extraction and ultra-performance liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography A,2011(42):7 608-7 614.
[12]Dolliver H,Kumar K,Gupta S. Sulfamethazine uptake by plants from manure-amended soil[J]. Journal of Environment Quality,2007,36(4):1 224-1 229.
[13]吴小莲,向垒,莫测辉,等.超高效液相色谱-电喷雾串联质谱测定蔬菜中喹诺酮类抗生素[J].分析化学,2013,41(6):876-881.
[2]Dosogne H,Meyer E,Sturk A,et al. Effect of enrofloxacin treatment on plasma endotoxin during bovine Escherichia colimastitis[J]. Inflammation Research, 2002, 51(4):201-205.
[3]Metcalfe C D,Miao X S,Koenig B G,et al. Distribution of acidic and neutral drugs in surface waters near sewage treatment plants in the lower Great Lakes, Canada[J].Environmental Toxicology and Chemistry,2003,22(12):2 881-2 890.
[4]Vieno N, Tuhkanen T, Kronberg L. Elimination of pharmaceuticals in sewage treatment plants in Finland[J].Water Research,2007,41(5):1 001-1 012.
[5]Aust M O,Godlinski F,Travis G R,et al. Distribution of sulfamethazine,chlortetracycline and tylosin in manure and soil of Canadian feedlots after subtherapeutic use in cattle[J]. Environmental Pollution,2008(3):1 240-1251.
[6]Karci A, Balcioglu I A. Investigation of the tetracycline,sulfonamide,and fluoroquinolone antimicrobial compounds in animal manure and agricultural soils in Turkey[J].Science of the Total Environment,2009(16):4 652-4 664.
[7]张慧敏,章明奎,顾国平.浙北地区畜禽粪便和农田土壤中四环素类抗生素残留[J].生态与农村环境学报,2008(3):69-73.
[8]潘杰平.浅谈兽药残留对食品安全的影响[J].中国动物保健,2018,20(5):8-9.
[9]农业部畜牧兽医局.农业部发布动物性食品中兽药最高残留限量[J].中国兽药杂志,2003,25(2):5-11.
[10]刘佳佳,金芬,佘永新,等.液相色谱-串联质谱法测定牛奶中5种多肽类抗生素[J].分析化学,2011,39(5):652-657.
[11]Herreraherrera A V,Hernándezborges J,Rodríguezdelgado M A,et al. Determination of quinolone residues in infant and young children powdered milk combining solidphase extraction and ultra-performance liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography A,2011(42):7 608-7 614.
[12]Dolliver H,Kumar K,Gupta S. Sulfamethazine uptake by plants from manure-amended soil[J]. Journal of Environment Quality,2007,36(4):1 224-1 229.
[13]吴小莲,向垒,莫测辉,等.超高效液相色谱-电喷雾串联质谱测定蔬菜中喹诺酮类抗生素[J].分析化学,2013,41(6):876-881.