分散固相萃取-超高效液相色谱-串联质谱检测水产品中14种喹诺酮类药物

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。

Determination of 14 Quinolone Antibiotics in Aquatic Products by Dispersive Solid-phase Extraction and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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.