干旱区生态环境知识资源中心(Arid): 超高效液相色谱-串联质谱法测定沼肥中六种喹诺酮类抗生素

Arid

	超高效液相色谱-串联质谱法测定沼肥中六种喹诺酮类抗生素
其他题名	Determination of Six Quinolones Antibiotics in Biogas Manures by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry
	张敏 1; 张俊 1; 付海滨 2; 刘庆玉 1; 李金洋 1
来源期刊	沈阳农业大学学报
ISSN	1000-1700
出版年	2018
卷号	49 期号:4 页码:486-490
中文摘要	为研究和优化沼肥中喹诺酮类抗生素残留的检测,利用超高效液相色谱-串联质谱法(UPLC-/MS/MS)建立了沼肥中6种喹诺酮类抗生素兽药(恩诺沙星、诺氟沙星、环丙沙星、氧氟沙星、噁喹酸、氟甲喹)残留的测定方法。样品经McIlvaine-Na_2 EDTA缓冲液和甲醇-乙腈(体积比1∶1)溶液提取,提取液经Oasis HLB固相萃取柱净化,采用Waters Acquity UPLC BEN C_(18)柱(50mm* 2.1mm,1.7mum)进行分离,以甲醇和0.2%甲酸水溶液为流动相进行梯度洗脱。采用超高效液相色谱柱进行分离,在采用电喷雾正电离源和多反应监测(MRM)模式下,用四极杆串联质谱仪进行定性和定量分析,标准曲线外标法定量。结果表明:6种喹诺酮类抗生素浓度为0.01~5.0mug·mL~(-1)时线性良好,相关系数(r)均大于0.9979,方法在0.01,0.05,0.5,2.0mg·kg~(-1)添加水平下,恩诺沙星、诺氟沙星、环丙沙星、氧氟沙星、噁喹酸、氟甲喹的回收率分别为78.5%~91.2%、73.8%~87.5%、73.5%~85.1%、72.6%~86.2%、72.5%~ 82.6%、73.5%~89.9%,相对标准偏差为3.78%~10.6%。6种喹诺酮类抗生素的检出限为0.5~1.1mug·kg~(-1),定量下限为1.7~3.6mug·kg~(-1)。说明该方法重现性良好,灵敏度、回收率高,检测时间短,适用于沼肥中6种喹诺酮类抗生素残留检测。
英文摘要	A method for the analysis of six quinolones, including enrofloxacin (ENR), norfloxacin (NOR), ciprofloxacin (CIP), ofloxacin (OFL), oxolinic acid (OA) and flumequine (FLU) , residue in biogas manures was developed based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were extracted with McIlvaine-Na_2 EDTA buffer and methanol-acetonitrile(1∶1,V/V) solution. Extraction liquid was purified by an Oasis HLB SPE column. The analytes were separated on a Waters Acquity C_(18) column. The mobile phase was 0.2% formic acid(V/V) and methanol in gradient elution. Qualitative and quantitative analyses were carried out by a triple quadrupole mass spectrometer equipped with an electrospray ionization source that operated in the multiple reaction monitoring mode (MRM). External standard method was adopted as the quantitative method. The calibration curves showed good linearity within the concentrations of 0.01-5.0mug·mL~(-1) with the correlation coefficients r> 0.993. The recoveries of ENR, NOR, CIP, OFL, OA and FLU were 78.5%-91.2%, 73.8%-87.5%, 73.5%-85.1%, 72.6%-86.2%, 72.5%-82.6% , 73.5%-89.9% , respectively, at the four spiked levels of 0.01, 0.05, 0.5, 2.0mug·kg~(-1). The relative standard deviations were both less than 3.78%-10.6%. The detected limits (LOD) ranged from 0.5mug·kg~(-1) to 1.1mug·kg~(-1), limit of quantification (LOQ) ranged from 1.7mug·kg~(-1) to 3.6mug·kg~(-1). It is concluded that this method can be successfully applied to the determination of 6 quinolones in biogas manures with good reproducibility, high sensitivity, high recovery rate and short analysis time.
中文关键词	喹诺酮类抗生素 ; 高效液相色谱-串联质谱法 ; 沼肥 ; 固相萃取
英文关键词	quinolones antibiotics ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) biogas manures SPE
语种	中文
国家	中国
收录类别	CSCD
WOS类目	AGRICULTURE MULTIDISCIPLINARY
WOS研究方向	Agriculture
CSCD记录号	CSCD:6312311
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/238063
作者单位	1.沈阳农业大学工程学院, 沈阳, 辽宁 110161, 中国; 2.沈阳出入境检验检疫局技术中心, 沈阳, 辽宁 110016, 中国
推荐引用方式 GB/T 7714	张敏,张俊,付海滨,等. 超高效液相色谱-串联质谱法测定沼肥中六种喹诺酮类抗生素[J],2018,49(4):486-490.
APA	张敏,张俊,付海滨,刘庆玉,&李金洋.(2018).超高效液相色谱-串联质谱法测定沼肥中六种喹诺酮类抗生素.沈阳农业大学学报,49(4),486-490.
MLA	张敏,et al."超高效液相色谱-串联质谱法测定沼肥中六种喹诺酮类抗生素".沈阳农业大学学报 49.4(2018):486-490.