干旱区生态环境知识资源中心(Arid): 超高效液相色谱-高分辨四级杆飞行时间质谱法快速筛查乳制品中磺胺类与氟喹诺酮类药物

Arid

	超高效液相色谱-高分辨四级杆飞行时间质谱法快速筛查乳制品中磺胺类与氟喹诺酮类药物
其他题名	Rapid Screening of Fluoroquinolones and Sulfonamides in Dairy Products Using Ultra Performance Liquid Chromatography Coupled to High Resolution Quadrupole Time-of-Flight Mass Spectrometry
	孟哲 1; 石志红 2; 吕运开 3; 孙汉文 3
来源期刊	分析化学
ISSN	0253-3820
出版年	2014
卷号	42 期号:10 页码:1493-1500
中文摘要	利用超高效液相色谱-高分辨四级杆飞行时间质谱联用技术,建立了一种快速筛查乳制品中8种氟喹诺酮5种磺胺类药物及其4种乙酰化代谢物的新方法。采用乙腈-20%三氯乙酸溶液(100:1,V/V,pH2.0)作溶剂和Oasis HLB固相萃取载体作吸附剂,实现了牛奶样品中17种目标物的同时提取和有效净化。利用MassLynx Chromlynx 软件建立了这17种分析物的数据库。以Full Scan/MSE进行定性筛查和定量检测。4种代谢物在10~2000mug/L范围内和其它分析物在0.5~100mug/L范围内,其基质匹配内标校准曲线呈现良好的线性(R2>0.983)。氟喹诺酮的定量限为0.5~0.8mug/kg,磺胺类药物及代谢物的定量限为0.5~13.0mug/kg。在3个添加水平分析物的平均回收率(69%~92%)在职业分析化学家协会(AOAC)提出的允许范围之内,相对标准偏差均小于15%。本方法快速而灵敏,成功用于乳制品中抗生素及其代谢物的筛查、确认和定量分析。所研究的每种药物及代谢物残留均低于有关的最高残留限量(MRLs),但某些乳制品中其总残留量已超过最高残留限量。
英文摘要	A novel analytical method employing ultra performance liquid chromatography-quadrupole-time-offlight mass spectrometry (UPLC-Q-TOF/ MS) was developed for the rapid screening of eight fluoroquinolones(FQs), five sulfonamides (SAs) and four acetyled metabolites in dairy products. The simultaneous extraction and effective cleanup for seventeen target analytes in dairy product samples were achieved with acetonitrile- 20% trichloroacetic acid (100: 1, V / V, pH 2) as solvent and Oasis HLB SPE cartridges as sorbent. Using MassLynx Chromalynx Software, a database for 17 target analytes was established. Qualitatively screening and quantitative analysis were carried out by full scan/ MS~E mode. The matrix-matched internal standard chalibration curves showed a good linearity (R~2 >0. 983) in the ranges of 10-2000 mug/ L for metabolites and 0. 5-100 mug/ L for other all antibioties. The limits of quantification were in the range of 0. 5-0. 8 mug/ kg for FQs and 0. 5-13. 0 mug/ kg for SAs and related metabolites. The average recoveries at three spiked levels were in the range of 69% -92%, which is within the acceptable range proposed by Association of Official Analytical Chemists (AOAC). The relative standard deviation was less than 15%. This novel approach had high speed and sensitivity, and was successfully applied to the screening, confirmation and quantification analysis of dairy products. The content of each analyte residue was much lower than the maximum residue limits (MRLs), but total content of multiresidue in some dairy product samples were more than the MRLs.
中文关键词	氟喹诺酮类 ; 磺胺类 ; 超高效液相色谱 ; 高分辨质谱 ; 乳制品
英文关键词	Fluoroquinolones Sulphonamides Ultra performance liquid chromatography High resolution mass spectrometry Dairy products
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY MULTIDISCIPLINARY
WOS研究方向	Chemistry
CSCD记录号	CSCD:5268671
来源机构	宁夏大学
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/231040
作者单位	1.河北大学化学与环境科学学院, 河北省分析科学技术实验室;;宁夏能源化工重点实验室, 保定, 河北 071002, 中国; 2.宁夏大学, 宁夏能源化工重点实验室, 银川, 宁夏 753200, 中国; 3.河北大学化学与环境科学学院, 河北省分析科学技术实验室, 保定, 河北 071002, 中国
推荐引用方式 GB/T 7714	孟哲,石志红,吕运开,等. 超高效液相色谱-高分辨四级杆飞行时间质谱法快速筛查乳制品中磺胺类与氟喹诺酮类药物[J]. 宁夏大学,2014,42(10):1493-1500.
APA	孟哲,石志红,吕运开,&孙汉文.(2014).超高效液相色谱-高分辨四级杆飞行时间质谱法快速筛查乳制品中磺胺类与氟喹诺酮类药物.分析化学,42(10),1493-1500.
MLA	孟哲,et al."超高效液相色谱-高分辨四级杆飞行时间质谱法快速筛查乳制品中磺胺类与氟喹诺酮类药物".分析化学 42.10(2014):1493-1500.