干旱区生态环境知识资源中心(Arid): 高效液相色谱-串联质谱法测定废水中5种喹诺酮类抗生素

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	高效液相色谱-串联质谱法测定废水中5种喹诺酮类抗生素
其他题名	Determination of Five Fluoroquinolone Antibiotics in Wastewater by High Performance Liquid Chromatography-Tandem Mass Spectrometry
	姚倩钰 1; 贺德春 2; 龚道新 1; 丁紫荣 2; 赵波 2; 张漫雯 2; 黎玉清 2
来源期刊	中国环境监测
ISSN	1002-6002
出版年	2017
卷号	33 期号:3 页码:139-146
中文摘要	建立高浓度有机废水中5种喹诺酮类抗生素的高效液相色谱-串联质谱测定方法。水样经HLB固相萃取小柱富集净化,12 ml甲醇洗脱、浓缩并加入内标溶液后,定容至1 mL待测。以C_(18)柱为分离柱,含0.01%甲酸的甲醇-含0.01%甲酸的水溶液为流动相,目标物质在10 min内分离。在0.25 ~ 1 250 ng/mL范围内,目标物质线性关系良好(R~2 >0.99)。基质加标试验结果表明,纯水中的回收率为61.40% ~91.92%,废水中的回收率为54.92% ~101.87%,检出限为0.25~2.5 ng/L,方法定量限为0.36~3.99 ng/L。应用该方法对21家猪场的64份废水样品进行分析,5种喹诺酮类抗生素的检出频率为47% ~95%,平均检出浓度为980~5 734 ng/L。该方法快速、准确,适用于高浓度有机废水中喹诺酮类抗生素的同时测定。
英文摘要	A method was established for determination of 5 fluoroquinolone antibiotics in high concentration of organic wastewater using solid phase extraction ( SPE) followed by high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/ MS) in this paper. Aqueous samples were developed with Oasis HLB solid-phase extraction ( SPE) cartridges and the targeted antibiotics were subsequently eluted by 12 mL methanol. After concentration, the elutes were added internal standards and determined by HPLC-MS/MS equipped with a reverse-phase C18 column. The results of method development showed that the 5 kinds of fluoroquinolone could be efficiently separated within 10 minutes by HPLC-MSMS ; the calibration curve ranged 0.25-1 250 ng/mL and showed high relationship ( R2 > 0.99 ). The recoveries for all analytes in pure water matrices were above 60%,and the recoveries of target compounds in real wastewater samples ranged 54.92% -101.87% ; detection limits varied between 0.25-2.5 ng/L and quantization limits were 0.36-3.99 ng/L. The presented method was successfully applied to quantify the five fluoroquinolones in 64 wastewater samples from 21 pig farms. The detection frequency of five quinolones in real samples was 47% -95% and the average detection concentration was found to be 980 to 5 734 ng/L. All the results indicate that this method is suitable for rapid determination of fluoroquinolone antibiotics in high concentration of organic wastewater.
中文关键词	高效液相色谱-串联质谱 ; 固相萃取 ; 废水 ; 喹诺酮类抗生素
英文关键词	high performance liquid chromatography-tandem mass spectrometry solid phase extraction wastewater fluoroquinolone antibiotics
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:6053820
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/237007
作者单位	1.湖南农业大学资源环境学院, 长沙, 湖南 410000, 中国; 2.环境保护部华南环境科学研究所, 广州, 广东 510000, 中国
推荐引用方式 GB/T 7714	姚倩钰,贺德春,龚道新,等. 高效液相色谱-串联质谱法测定废水中5种喹诺酮类抗生素[J],2017,33(3):139-146.
APA	姚倩钰.,贺德春.,龚道新.,丁紫荣.,赵波.,...&黎玉清.(2017).高效液相色谱-串联质谱法测定废水中5种喹诺酮类抗生素.中国环境监测,33(3),139-146.
MLA	姚倩钰,et al."高效液相色谱-串联质谱法测定废水中5种喹诺酮类抗生素".中国环境监测 33.3(2017):139-146.