| 刘 博,薛南冬,杨 兵,龚道新,李发生,张石磊,周玲莉,孟 磊,陈宣宇,燕云仲.高效液相色谱-荧光检测法同时分析鸡粪中六种氟喹诺酮类抗生素[J].农业环境科学学报,2014,33(5):1050-1056. |
| 高效液相色谱-荧光检测法同时分析鸡粪中六种氟喹诺酮类抗生素 |
| Simultaneous Determination of Six Fluoroquinolones in Chicken Manures by High Performance Liquid Chromatography with Fluorescence Detection |
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| DOI：10.11654/jaes.2014.05.031 |
| 中文关键词: 氟喹诺酮类抗生素 固相萃取-高效液相色谱荧光检测法（SPE-HPLC/FLD） 禽畜粪便 分析方法 |
| 英文关键词: fluoroquinolones（FQs） solid-phase extraction-high performance liquid chromatography with fluorescence detection livestock and poultry excrement analytical method |
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| 摘要点击次数: 2501 |
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| 中文摘要: |
| 通过对样品预处理过程优化、提取剂与洗脱剂的筛选和检测色谱条件优化，建立了基于固相萃取-高效液相色谱荧光检测法分析鸡粪中6种氟喹诺酮类（ＦＱｓ）的检测方法。该方法选用Mcllvaine-Na2EDTA缓冲液∶乙腈（1∶1，V/V）（pH=2）作为提取剂，超声提取时间15 min，经HLB固相柱净化，选用甲醇为洗脱剂，浓缩后用HPLC/FLD检测，采用乙腈/0.7%磷酸作为流动相。FQs在0.01～1.0 mg·kg-1浓度范围内呈现良好线性关系，R2为0.996 9～0.999 9。加标（浓度水平0.01、0.5、1.0 mg·kg-1干重）回收率达76.7%～106.7%，相对标准偏差0.7%～14.4%（n=4）。方法检出限为0.002～0.022 mg·kg-1，方法定量限为0.006 8～0.074 mg·kg-1。应用该方法对北京地区5个养鸡场内鸡粪样品中6种FQs进行分析，检出浓度为ND～1.13 mg·kg-1。 |
| 英文摘要: |
| An analytical method for simultaneous determination of six fluoroquinolones（FQs） in chicken manures based on solid-phase extraction and high performance liquid chromatography with a fluorescence detection（HPLC/FLD） was developed in the current study. Samples were ultrasonically extracted in Mcllvaine-Na2EDTA buffer/acetonitrile（1∶1）（pH=2） for 15 min. The extract was cleaned by a HLB solid-phase extraction column, and then eluted with methanol solvent. The fluoroquinolones in the extract were determined by HPLC/FLD with acetonitrile/0.7% phosphate as mobile phase. In a concentration range of 0.01~1.0 mg·kg-1, R2 of calibration was greater than 0.99. The average percent recoveries ranged from 76.7% to 106.7% for six compounds in chicken manure samples at three different spiked levels（0.1, 0.5 mg·kg-1 and 1.0 mg·kg-1）. The detection limits（LOD） were from 0.002 mg·kg-1 to 0.022 mg·kg-1, and limit of quantification（LOQ） from 0.006 8 mg·kg-1 to 0.074 mg·kg-1. This method was used to analyze six FQs in chicken manures collected from 5 chicken farms in Beijing. All six FQs were detected in most samples, with concentrations ranging from LOD to 1.13 mg·kg-1. |
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