高效液相色谱法测定淡水渔业用水中诺氟沙星、环丙沙星、恩诺沙星残留
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摘要
该文采用高效液相色谱—荧光法检测淡水渔业用水中诺氟沙星、环丙沙星和恩诺沙星3种喹诺酮类抗生素药物的残留,建立了检测淡水渔业用水中喹诺酮类抗生素药物的方法。结果显示,诺氟沙星、环丙沙星和恩诺沙星的检出限(按S/N=3计)分别为2.5、1.0、2.5μg/L,定量限(按S/N=10计)分别为5、1、5μg/L。按1倍、5倍、10倍定量限进行加标回收,3种抗生素的平均回收率为76.6%～89.9%,相对标准偏差(RSD)在1.72%～8.43%。
The high performance liquid chromatography(HPLC)-fluorescence assay was adopted to detect norfloxacin, ciprofloxac, enrofloxacin residues in fishery water in the research, and the method for the determination of residues of three quinolones was developed. The results showed that the detection limit(S/N=3) of nor floxacin, ciprofloxac and enrofloxacin was 2.5 μg/L、1 μg/L and 2.5 μg/L, respectively; and the quantitative limit(S/N=10) was 5 μg/L、1 μg/L and 5μg/L, respectively. When adding a concentration of 1 times, 5 times, 10 times the limit of quantity, the average recovery was between 76.6% and 89.9% and the relative standard deviation was between 1.72% and 8.43%.
The high performance liquid chromatography(HPLC)-fluorescence assay was adopted to detect norfloxacin, ciprofloxac, enrofloxacin residues in fishery water in the research, and the method for the determination of residues of three quinolones was developed. The results showed that the detection limit(S/N=3) of nor floxacin, ciprofloxac and enrofloxacin was 2.5 μg/L、1 μg/L and 2.5 μg/L, respectively; and the quantitative limit(S/N=10) was 5 μg/L、1 μg/L and 5μg/L, respectively. When adding a concentration of 1 times, 5 times, 10 times the limit of quantity, the average recovery was between 76.6% and 89.9% and the relative standard deviation was between 1.72% and 8.43%.
引文
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[7]李佩佩,张小军,梅光明,等.超高效液相色谱-串联质谱检测养殖水体中喹诺酮类抗生素[J].浙江大学学报(理学版),2015,42(3):334-338.
[8]李佩佩,陈雪昌,张小军,等.高效液相色谱法检测水产品中氟奎诺酮类药物残留量方法的优化[J].中国渔业质量与标准,2012,2(2):84-88.
[9]杨金易,张燕,曾道平,等.基于QuEchERS前处理技术的水产品中喹诺酮类药物多残留ELISA检测方法的建立[J].食品工业科技,2015,36(01):292-298.
[10]柳爱春,刘超,张乐,等.免疫胶体金法快速检测水产品中喹诺酮类药物[J].浙江农业学报,2018,30(2):290-297.
[11]Dorival-Garcia,N,Zafra-Gomez,A,Navalon,A,et al.Removal of quinolone antibiotics from wastewaters by sorption and biological degradation in laboratory-scale membrane bioreactors[J].Science of the Total Environment,2013,442C:317-328.
[12]金钥,孙延斌,崔进,等.水产品中喹诺酮类和磺胺类兽药残留检测方法的建立[J].食品研究与开发,2016,37(19):122-127.
[2]杜鹃,赵红霞,陈景文.固相萃取-高效液相色谱-串联质谱法同时测定养殖海水中23种抗生素[J].色谱,2015,33(4):348-353.
[3]ChenY Sh,Cao Q M,Deng Sh B,et al.Determination of pharmaceuticals from various therapeutic classes in dewatered sludge by pressurized liquid extraction and high performance liquid chromatography and tandem mass spectrometry[J].International Journal of Environmental Analyticl Chemistry,2013,93(11):1159-1173.
[4]Wollenbrger L,Halling-s*rensen B,Kusk KO.Acute and chronic toxicity of veterinary antibiotics to Daphnia magna[J].Chemosphere,2000(40):723-730.
[5]杨守国,李兆新,王清印,等.高效液相色谱法检测海水养殖环境中喹诺酮类药物残留[J].渔业科学进展,2010,31(2):95-101.
[6]董晓,李兆新,孙晓杰,等.固相萃取-液相色谱串联质谱法同时测定养殖海水中17种喹诺酮类药物[J].渔业科学进展,2017,38(6):127-138.
[7]李佩佩,张小军,梅光明,等.超高效液相色谱-串联质谱检测养殖水体中喹诺酮类抗生素[J].浙江大学学报(理学版),2015,42(3):334-338.
[8]李佩佩,陈雪昌,张小军,等.高效液相色谱法检测水产品中氟奎诺酮类药物残留量方法的优化[J].中国渔业质量与标准,2012,2(2):84-88.
[9]杨金易,张燕,曾道平,等.基于QuEchERS前处理技术的水产品中喹诺酮类药物多残留ELISA检测方法的建立[J].食品工业科技,2015,36(01):292-298.
[10]柳爱春,刘超,张乐,等.免疫胶体金法快速检测水产品中喹诺酮类药物[J].浙江农业学报,2018,30(2):290-297.
[11]Dorival-Garcia,N,Zafra-Gomez,A,Navalon,A,et al.Removal of quinolone antibiotics from wastewaters by sorption and biological degradation in laboratory-scale membrane bioreactors[J].Science of the Total Environment,2013,442C:317-328.
[12]金钥,孙延斌,崔进,等.水产品中喹诺酮类和磺胺类兽药残留检测方法的建立[J].食品研究与开发,2016,37(19):122-127.