| 贺南南,管永祥,梁永红,吴昊,罗朝晖,赵海燕,顾祖丽.高效液相色谱-荧光检测法同时分析沼液中4种喹诺酮类抗生素[J].农业环境科学学报,2016,35(10):2034-2040. |
| 高效液相色谱-荧光检测法同时分析沼液中4种喹诺酮类抗生素 |
| Simultaneous determination of four fluoroquinolones in biogas slurry by high performance liquid chromatography with fluorescence detection |
| 投稿时间：2016-04-01 |
| DOI：10.11654/jaes.2016-0442 |
| 中文关键词: 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) 沼液 分析方法 |
| 英文关键词: fluoroquinolones solid-phase extraction-high performance liquid chromatography with fluorescence detection biogas slurry analytical method |
| 基金项目:国家水体污染控制与治理科技重大专项（2012ZX07101-009）；国家公益性行业（农业）科研专项（201303089） |
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| 中文摘要: |
| 通过对沼液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，建立了固相萃取-高效液相色谱-荧光检测法分析沼液中4种喹诺酮类抗生素（FQs）的检测方法。该方法选用Na2EDTA溶液作为提取剂，调节样品pH=4，漩涡混匀后经HLB固相萃取柱净化，选用6 mL甲醇为洗脱剂，浓缩后用高效液相色谱-荧光分析法（HPLC-FLD）检测，采用乙腈/0.01 mol·L-1四丁基溴化铵作为流动相，外标法定量。4种FQs在0.002~5.0 mg·L-1浓度范围内呈现良好线性关系，R2均大于0.990。样品在0.1、0.2、0.5、1.0、2.0、5.0 mg·L-1 6个添加水平下的平均回收率在80.4%~105.7%，相对标准偏差为1.0%~5.1%，方法的检出限为0.004~0.01 mg·L-1。应用该方法对南京地区分别以鸡粪、猪粪、牛粪为发酵原料的3个大中型沼气工程的沼液样品进行分析，4种喹诺酮类抗生素均被检出，检测浓度为5~204 μg·L-1，表明沼液中抗生素污染问题值得关注。 |
| 英文摘要: |
| An analytical method for simultaneous determination of four fluoroquinolones(FQs) in biogas slurry based on solid-phase extraction and high performance liquid chromatography with a fluorescence detection(HPLC/FLD) was developed in this study. The homogenized sample adjusted to pH=4 was extracted with Na2EDTA solution, purified by Oasis HLB solid phase extraction after vortexing, and eluted with 6 mL methanol solvent. The FQs in the extract were determined by HPLC/FLD with acetonitrile and 0.01 mol·L-1 tetrabutylammonium bromide as mobile phases. Quantitation was carried out using an external standard method. The standard curves for all the compounds were linear over the concentration ranges of 0.002 mg·L-1 to 5.0 mg·L-1 with all correlation coefficients above 0.990． The spiked recoveries at six levels of 0.1, 0.2, 0.5, 1.0, 2.0 mg·L-1 and 5.0 mg·L-1 were ranged from 80.4% to 105.7%, and the relatives standard deviations(RSD) were in the ranges of 1.0% to 5.1%. The limits of detection were from 0.004 mg·L-1 to 0.01 mg·L-1. This method was used to analyze four FQs in biogas slurry samples fermented with chicken dung, pig dung, and cow dung collected from 3 large and medium-sized biogas projects in Nanjing. Four FQs were detected in all samples, with concentrations ranging from 5 μg·L-1 to 204 μg·L-1, four kinds of FQs were detected. Therefore, antibiotic pollution problems in biogas slurry deserve attention. |
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