干旱区生态环境知识资源中心(Arid): SPE-UFLC-MS/MS法测定制药废水中四环素类抗生素

Arid

	SPE-UFLC-MS/MS法测定制药废水中四环素类抗生素
其他题名	Determination of Tetracyclines in Pharmaceutical Wastewater by Solid Phase Extraction-Ultra Fast Liquid Chromatography-Tandem Mass Spectrometry
	李再兴 1; 张非非 1; 左剑恶 2; 张敬轩 3; 李挥 3; 余忻 2; 剧盼盼 1
来源期刊	环境科学与技术
ISSN	1003-6504
出版年	2013
卷号	36 期号:7 页码:139-142
中文摘要	文章建立了利用固相萃取-超快速液相色谱-串联质谱(SPE-UFLC-MS/MS)测定制药废水中四环素类抗生素(土霉素、四环素和金霉素)残留的方法。水样经(30%硫酸锌+20%亚铁氰化钾)溶液作为沉淀剂沉淀蛋白质后,上清液采用Oasis HLB固相萃取柱富集和净化,以(0.1%甲酸溶液+乙腈)为流动相进行梯度洗脱,经Agilent ZORBAX SB C_(18)柱分离后,在串联质谱ES(I+)模式下进行MRM检测。该方法四环素类抗生素检出限(S/N=3时)0.02mug/L,3种目标物在0.010~1.0 mg/L范围内线性关系良好,线性相关系数在0.998 2~0.999 8之间。在0.20、0.40和0.60mug/L添加水平,各组分的回收率在80.8%~97.2%之间,相对标准偏差在5.31%~9.92%之间。该方法可满足制药废水中四环素类抗生素残留检测的要求。
英文摘要	A method based on solid phase extraction-ultra fast liquid chromatography-tandem mass spectrometry (SPEUFLC -MS/MS)was developed to determine tetracyclines such as xoytetracycline, tetracycline, chlortetracycline in pharmaceutical wastewater. Water samples were firstly purified through protein precipitation process with 30% zinc sulfate and 20% potassium ferrocyanide,and the tetracyclines was enriched and purified with Oasis HLB SPE,separated through Agilent ZORBAX SB C_(18) UFLC using 0.1% formic acid solution and acetonitrile as mobile phase,and detected by mass spectrometry in positive ion mode with multiple reaction monitoring using an electrospray ionization interface. The detection limit was 0.02 mug/L. The linear range was 0.010 to 1.0 mg/L,with a correlation coefficient of 0.998 2~0.999 8. The recoveries at the spiked concentration of 0.20,0.40 and 0.60 mug/L ranged from 80.8% to 97.2%,with a relative standard deviation from 5.31% to 9.92%. The procedure would provide a method for determination of tetracyclines in pharmaceutical wastewater.
中文关键词	四环素类抗生素 ; 超快速液相色谱-串联质谱 ; 固相萃取 ; 制药废水
英文关键词	tetracyclines ultra fast liquid chromatography -tandem mass spectrometry (UFLC -MS/MS) solid phase extraction(SPE) pharmaceutical wastewater
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:4898638
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/229794
作者单位	1.河北科技大学环境科学与工程学院, 石家庄, 河北 050018, 中国; 2.清华大学环境学院, 北京 100084, 中国; 3.国家环保产品质量监督检验中心, 石家庄, 河北 050051, 中国
推荐引用方式 GB/T 7714	李再兴,张非非,左剑恶,等. SPE-UFLC-MS/MS法测定制药废水中四环素类抗生素[J],2013,36(7):139-142.
APA	李再兴.,张非非.,左剑恶.,张敬轩.,李挥.,...&剧盼盼.(2013).SPE-UFLC-MS/MS法测定制药废水中四环素类抗生素.环境科学与技术,36(7),139-142.
MLA	李再兴,et al."SPE-UFLC-MS/MS法测定制药废水中四环素类抗生素".环境科学与技术 36.7(2013):139-142.