PDF(Pubmed)
Abstract：
The amount of macrolide (MAL) residues in aquatic products, including oleandomycin (OLD), erythromycin (ERM), clarithromycin (CLA), azithromycin (AZI), kitasamycin (KIT), josamycin (JOS), spiramycin (SPI), tilmicosin (TIL), tylosin (TYL), and roxithromycin (ROX), was determined using solid-phase extraction and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The residues were extracted with 1% ammonia acetonitrile solution and purified by neutral alumina adsorption. Chromatographic separation was completed on an ACQUITY UPLC BEH C18 column with acetonitrile-0.1% formic acid aqueous solution as the mobile phase, and mass spectrometry detection was performed by multiple reaction monitoring scanning with the positive mode in an electrospray ion source (ESI+). Five isotopically labeled compounds were used as internal standards for quality control purposes. The findings indicated that across the mass concentration span of 1.0-100 μg/L, there was a strong linear correlation (R2 > 0.99) between the concentration and instrumental response for the 10 MALs. The limit of detection of UPLC-MS/MS was 0.25-0.50 μg/kg, and the limit of quantitation was 0.5-1.0 μg/kg. The added recovery of blank matrix samples at standard gradient levels (1.0, 5.0, and 50.0 μg/kg) was 83.1-116.6%, and the intra-day precision and inter-day precisions were 3.7 and 13.8%, respectively. The method is simple and fast, with high accuracy and good repeatability, in line with the requirements for accurate qualitative and quantitative analysis of the residues for 10 MALs in aquatic products.
摘要：
水产品中大环内酯(MAL)残留量,包括oleandomycin（旧），红霉素（ERM），克拉霉素（CLA），阿奇霉素（AZI），Kitasamycin(KIT),交沙霉素（JOS），螺旋霉素（SPI），替米考星(TIL),泰乐菌素(TYL),和罗红霉素（ROX），使用固相萃取和超高效液相色谱-串联质谱(UPLC-MS/MS)进行测定。残余物用1%氨乙腈溶液提取,并通过中性氧化铝吸附纯化。在ACQUITYUPLCBEHC18柱上完成色谱分离，以乙腈-0.1%甲酸水溶液为流动相，和质谱检测是通过在电喷雾离子源（ESI）中使用正模式进行的多反应监测扫描进行的。五种同位素标记的化合物用作质量控制目的的内标。结果表明，在1.0-100μg/L的质量浓度范围内，10例MAL的浓度与仪器反应之间存在很强的线性相关(R2>0.99)。UPLC-MS/MS的检出限为0.25-0.50μg/kg,定量限为0.5-1.0μg/kg。空白基质样品在标准梯度水平(1.0、5.0和50.0μg/kg)下的添加回收率为83.1-116.6%,日内精度和日间精度分别为3.7%和13.8%，分别。该方法简单、快速，精度高，重复性好，符合水产品中10种MALs残留准确定性定量分析的要求。
