固相萃取-高效液相色谱法同时测定鸡粪中四环素类、喹诺酮类和磺胺类抗生素
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摘要
建立了一种高效、低成本的固相萃取-高效液相色谱(SPE-HPLC)同时测定鸡粪中6种常见抗生素(2种四环素类、2种喹诺酮类和2种磺胺类)的分析方法。样品经EDTA-McIlvaine缓冲液和有机混合提取液(甲醇-乙腈-丙酮,2∶2∶1, v/v/v)提取,过HLB固相萃取柱净化,甲醇-二氯甲烷(7∶3, v/v)洗脱,高效液相色谱-二极管阵列检测器测定,检测波长λ=270 nm,柱温32℃,流动相为乙腈-0.7%(v/v)磷酸水溶液。该方法在0.5～100 mg/L质量浓度范围内的标准曲线相关系数r~2在0.999 9～1之间,样品加标回收率在70.0%～116.3%之间,相对标准偏差为1.2%～16.6%。方法检出限为1.3～6.7μg/kg,定量限为3.5～9.2μg/kg。应用该方法对辽宁省抚顺市某养鸡场当天的鸡粪进行检测,诺氟沙星和恩诺沙星(喹诺酮类)含量为未检出～9.23 mg/kg和1.57～7.69 mg/kg,磺胺二甲嘧啶(磺胺类)含量为2.02～13.05 mg/kg,磺胺甲恶唑、土霉素和四环素未测出。
A highly efficient and economic method for the simultaneous determination of six common antibiotics(two tetracyclines, two quinolones, and two sulfonamides) in chicken manure was developed by using solid-phase extraction and high performance liquid chromatography(SPE-HPLC). The samples were extracted by using a mixture of the EDTA-McIlvaine buffer and a mixed organic extractant(methanol-acetonitrile-acetone, 2∶2∶1, v/v/v), cleaned by a hydrophile-lipophile balance(HLB) cartridge, eluted by methanol-dichloromethane(7∶3, v/v), and separated by HPLC with an acetonitrile-0.7%(v/v) H_3PO_4 aqueous solution as the mobile phase. The detection wavelength and temperature of the chromatographic column were 270 nm and 32 ℃, respectively. All antibiotics showed great linear relationships in the range of 0.5-100 mg/L; the correlation coefficients(r~2) of the standard curves were between 0.999 9 and 1; the recoveries of antibiotics were between 70.0% and 116.3%; and the relative standard deviations were between 1.2% and 16.6%. The limits of detection were 1.3-6.7 μg/kg; and the limits of quantity were 3.5-9.2 μg/kg. This method was used to detect antibiotics in chicken manure from a hennery in Fushun, Liaoning Province. The contents of norfloxacin and enrofloxacin(quinolones) were from not detected to 9.23 mg/kg and 1.57-7.69 mg/kg, respectively, that of sulfamethazine(sulfonamides) were 2.02-13.05 mg/kg, while sulfamethoxazole, oxytetracycline, and tetracycline were undetectable.
A highly efficient and economic method for the simultaneous determination of six common antibiotics(two tetracyclines, two quinolones, and two sulfonamides) in chicken manure was developed by using solid-phase extraction and high performance liquid chromatography(SPE-HPLC). The samples were extracted by using a mixture of the EDTA-McIlvaine buffer and a mixed organic extractant(methanol-acetonitrile-acetone, 2∶2∶1, v/v/v), cleaned by a hydrophile-lipophile balance(HLB) cartridge, eluted by methanol-dichloromethane(7∶3, v/v), and separated by HPLC with an acetonitrile-0.7%(v/v) H_3PO_4 aqueous solution as the mobile phase. The detection wavelength and temperature of the chromatographic column were 270 nm and 32 ℃, respectively. All antibiotics showed great linear relationships in the range of 0.5-100 mg/L; the correlation coefficients(r~2) of the standard curves were between 0.999 9 and 1; the recoveries of antibiotics were between 70.0% and 116.3%; and the relative standard deviations were between 1.2% and 16.6%. The limits of detection were 1.3-6.7 μg/kg; and the limits of quantity were 3.5-9.2 μg/kg. This method was used to detect antibiotics in chicken manure from a hennery in Fushun, Liaoning Province. The contents of norfloxacin and enrofloxacin(quinolones) were from not detected to 9.23 mg/kg and 1.57-7.69 mg/kg, respectively, that of sulfamethazine(sulfonamides) were 2.02-13.05 mg/kg, while sulfamethoxazole, oxytetracycline, and tetracycline were undetectable.
引文
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[10]Petrie B,Barden R,Kasprzyk-Hordern B.Water Res,2015,72:3
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[13]Zhu F,Ji W L,Ruan L P,et al.Chinese Journal chromatography,2016,34(3):299朱峰,吉文亮,阮丽萍,等.色谱,2016,34(3):299
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[15]Orso D,Floriano L,Ribeiro L C,et al.Food Anal Method,2016,9(6):1638
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[23]Wang R,Wei Y S.Journal of Agro-Environment Science,2013,9(9):1705王瑞,魏源送.农业环境科学学报,2013,9(9):1705
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[28]Samanidou V F,Christodoulou E A,Papadoyannis I N.JSep Sci,2015,28(4):325
[29]Schneider M J,Braden S E,Reyes-Herrera I,et al.J Chromatogr B,2007,846(1):8
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