摘要
采用基质固相分散的前处理技术,建立一种超高效液相色谱-串联质谱同时检测水产品中14种喹诺酮类药物的分析方法。样品用5%甲酸-乙腈溶液提取和盐析剂盐析后加入N-丙基乙二胺和十八烷基键合硅胶吸附剂(C18)净化剂进行基质固相分散净化,氮吹复溶后经Waters ACQUITY UPLC BEH C18柱(50 mm×2.1 mm,1.7μm)分离,以0.2%甲酸溶液和甲醇为流动相梯度洗脱,采用电喷雾离子源正离子多反应监测模式测定,外标法定量。14种药物在0.50~20.0μg/L质量浓度范围内呈良好线性,线性相关系数不小于0.995。方法检出限为0.4~1.0μg/kg,定量限为1.0~3.0μg/kg。14种药物在3个加标水平下的平均回收率为82%~90%,相对标准偏差(n=5)均小于11.0%。本方法简便快速、灵敏度高、实用性强,可作为水产品中14种喹诺酮类药物残留的快速确证和定量分析。
A method for the simultaneous analysis of 14 quinolone(QN) residues in aquatic products by dispersive solidphase extraction and liquid chromatography-tandem mass spectrometry(UPLC-MS-MS) was established. The sample was extracted with acetonitrile(containing 5% formic acid) and followed by salting-out. Clean up of the extracts was performed using PSA and C18 during the dispersive solid-phase extraction procedure. After evaporated to dryness under a stream of nitrogen, the analytes were then separated on a Waters ACQUITY UPLCTM BEH C18 column(50 mm × 2.1 mm, 1.7 μm) using binary mobile phase gradient with water containing 0.2% formic acid and methanol. The targeted compounds were detected under a multiple reaction monitoring(MRM) mode and quantified by an external standard method. The linearity of all 14 QNs in the range from 0.50 to 20.0 μg/L exhibited correlation coefficients greater than 0.995. The limits of detection(LOD) and the limits of quantification(LOQ) were 0.4–1.0 and 1.0–3.0 μg/kg, respectively. The average recoveries of 14 QNs at three level spiked concentrations ranged from 82% to 90%, with relative standard deviations(n = 5) less than 11.0%. This method was simple, rapid, sensitive and reliable, and could be applied to determine 14 QNs in aquatic products.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2014年第24期265-270,共6页
Food Science
基金
浙江省重点科技创新团队项目(2010R50028)
浙江省科技计划项目(2013C37072
2012F20026)
关键词
基质固相分散
超高效液相色谱-串联质谱
水产品
喹诺酮类药物
dispersive solid-phase extraction
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS)
aquatic products
quinolones
