干旱区生态环境知识资源中心(Arid): 超高效液相色谱-三重四极杆质谱法测定地表水和废水中的19种磺胺类抗生素

Arid

	超高效液相色谱-三重四极杆质谱法测定地表水和废水中的19种磺胺类抗生素
其他题名	Determination of 19Sulfonamide Antibiotics in Suface Water and Waste Water by Ultra Hight Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry
	郑璇; 张晓岭; 邹家素; 孙静
来源期刊	理化检验. B, 化学分册
ISSN	1001-4020
出版年	2018
卷号	54 期号:6 页码:680-687
中文摘要	样品采集于棕色高密度聚乙烯瓶或玻璃瓶中,尽快进行前处理,于4℃保存不超过7 d。水样经0.45mum滤膜过滤,移取1L,加入1 g的Na2EDTA,用0.1 mol·L~(-1) NaOH溶液调节样品溶液的pH至6.0,采用OASIS HLB固相萃取柱对待测物进行富集萃取,用10 mL水洗涤小柱,真空干燥10 min,再用10 mL甲醇洗脱待测物,收集洗脱液,氮吹浓缩至干,用初始流动相定容至1 mL,加入1.00 mg·L~(-1)的内标混合溶液50muL,过0.20mum亲水性聚丙烯滤膜后,采用HYPERSIL GOLD C18色谱柱(100 mm*2.1 mm,1.9mum)分离待测物,以0.05%(体积分数)甲酸溶液和甲醇为流动相进行梯度洗脱,质谱分析中采用电喷雾正离子源和多反应监测模式。19种磺胺类抗生素的线性范围均为2.0~100mug·L~(-1),检出限(3.143 s)在0.6~2.0 ng·L~(-1)之间。加标回收率为77.6%~134%,测定值的相对标准偏差为1.9%~11%。方法应用于测定地表水和养殖企业废水中的抗生素残留,地表水中仅检出两种目标物,质量浓度分别为2.60,2.10 ng·L~(-1),养殖企业废水检出7种目标物,质量浓度在2.82~34.3 ng·L~(-1)之间。
英文摘要	The water samples were collected in brown high-density polyethylene bottles or glass bottles and pretreated as soon as possible,and stored at 4℃for no more than 7 days.The collected sample was filtered through a 0.45mum filter and 1 g of Na2EDTA was added into 1Lof the sample.The pH of the sample solution was adjusted to 6.0 with 0.1 mol·L~(-1) NaOH solution,and the OASIS HLB solid phase extraction column was used for enrichment and extraction of the analytes.After the column was washed with 10 mL of water and dried in vacuum for 10 min,the analytes was eluted with 10 mL of methanol and the eluate was collected and concentrated by nitrogen-blowing to dryness.The residue was diluted to 1 mL with the initial mobile phase,and 50muL of 1.00 mg·L~(-1) mixed internal standard solution was added,then the solution was filtred with 0.20mum hydrophilic polypropylene membrane.The analytes were seperated on a HYPERSIL GOLD C18 column(100 mm*2.1 mm, 1.9mum),with 0.05% (volume fraction)formic acid solution and methanol as the mobile phase for gradient elution. Electrospray positive ion source and multiple reaction monitoring mode were used in mass spectrometry analysis. Linearity range of 19 sulfonamide antibiotics was same 2.0-100mug·L~(-1),with detection limits(3.143 s)in the range of 0.6-2.0 ng·L~(-1).Values of recovery obtained by standard addition method ranged from 77.6% to 134%,and RSDs(n=6)ranged from 1.9%to 11%.The method was applied to the determination of antibiotic residues in the surface water and wastewater from a farming enterprise,only two targets with mass concentrations of 2.60,2.10 ng·L~(-1) were found in the surface water,and 7 targets with mass concentrations in the range of 2.82-34.3 ng·L~(-1) were found in the wastewater from a farming enterprise.
中文关键词	超高效液相色谱-三重四极杆质谱法 ; 磺胺 ; 抗生素 ; 地表水 ; 废水
英文关键词	ultra hight performance liquid chromatography-tripe quadrupole mass spectrometry sulfonamide antibiotic surface water waste water
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY ANALYTICAL
WOS研究方向	Chemistry
CSCD记录号	CSCD:6269686
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/237910
作者单位	重庆市生态环境监测中心, 有机污染物环境化学行为与生态毒理重庆市重点试验室, 重庆 401147, 中国
推荐引用方式 GB/T 7714	郑璇,张晓岭,邹家素,等. 超高效液相色谱-三重四极杆质谱法测定地表水和废水中的19种磺胺类抗生素[J],2018,54(6):680-687.
APA	郑璇,张晓岭,邹家素,&孙静.(2018).超高效液相色谱-三重四极杆质谱法测定地表水和废水中的19种磺胺类抗生素.理化检验. B, 化学分册,54(6),680-687.
MLA	郑璇,et al."超高效液相色谱-三重四极杆质谱法测定地表水和废水中的19种磺胺类抗生素".理化检验. B, 化学分册 54.6(2018):680-687.