干旱区生态环境知识资源中心(Arid): 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

Arid

	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
其他题名	Simultaneous determination of four fluoroquinolones in biogas slurry by high performance liquid chromatography with fluorescence detection
	贺南南 1; 管永祥 2; 梁永红 2; 吴昊 3; 罗朝晖 1; 赵海燕 1; 顾祖丽 1
来源期刊	农业环境科学学报
ISSN	1672-2043
出版年	2016
卷号	35 期号:10 页码:2034-2040
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Na_2EDTA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,R~2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 mug·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 Na_2EDTA 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 mug·L~(-1) to 204 mug·L~(-1), four kinds of FQs were detected. Therefore, antibiotic pollution problems in biogas slurry deserve attention.
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
语种	中文
国家	中国
收录类别	CSCD
WOS类目	ENVIRONMENTAL SCIENCES
WOS研究方向	Environmental Sciences & Ecology
CSCD记录号	CSCD:5835421
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/234650
作者单位	1.南京农业大学资源与环境科学学院, 南京, 江苏 210095, 中国; 2.江苏省耕地质量与农业环境保护站, 南京, 江苏 210036, 中国; 3.江苏省农业环境监测与保护站, 南京, 江苏 210036, 中国
推荐引用方式 GB/T 7714	贺南南,管永祥,梁永红,等. 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],2016,35(10):2034-2040.
APA	贺南南.,管永祥.,梁永红.,吴昊.,罗朝晖.,...&顾祖丽.(2016).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.农业环境科学学报,35(10),2034-2040.
MLA	贺南南,et al."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".农业环境科学学报 35.10(2016):2034-2040.