Canadian Food Inspection Agency, Dartmouth, N.S., Canada.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2009 Jan;26(1):39-46. doi: 10.1080/02652030802189757.
An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of fluoroquinolones-ciprofloxacin (CIPRO), danofloxacin (DANO), enrofloxacin (ENRO) and sarafloxacin (SARA)-in aquaculture products, specifically salmon, shrimp and tilapia. After initial sample extraction with an acidic acetonitrile solution, the extract was diluted with dichloromethane and centrifuged, then an aliquot was concentrated and applied to a C18 solid-phase extraction cartridge and concentrated for a second time. The resultant residue was dissolved in acetonitrile, diluted with water, and then further defatted with hexane. The fluoroquinolone residues were determined by UPLC with an HSS T3 C18 reverse-phase column using an ammonium hydroxide-formic acid buffer in an acetonitrile gradient with MS/MS detection using multiple reaction monitoring. Average recoveries for salmon tissue ranged from 73% for DANO to 95% for SARA, for shrimp from 71% for DANO to 109% for SARA, and from 62% for DANO to 111% for SARA in tilapia, fortified at the 1.0 ng g(-1) level. Standard curves were linear between 0.002 and 0.5 ng injected for all compounds. Detection limits of 0.2 ng g(-1) for CIPRO, DANO, ENRO, and SARA were easily obtainable. The operational errors, interferences, and recoveries for fortified samples demonstrate that this described method is suitable for routine use in a regulatory programme. The recommended method is simple, rapid, specific and reliable for the routine monitoring of fluoroquinolone residues in aquatic species such as salmon, tilapia and shrimp.
建立了一种超高效液相色谱-串联质谱法（UPLC-MS/MS），用于测定养殖产品（三文鱼、虾和罗非鱼）中的氟喹诺酮类药物-环丙沙星（CIPRO）、丹诺沙星（DANO）、恩诺沙星（ENRO）和沙拉沙星（SARA）。样品经酸性乙腈溶液提取后，用二氯甲烷稀释并离心，然后将一部分样品浓缩，再用 C18 固相萃取小柱浓缩，得到的残渣用乙腈溶解，用水稀释，然后用正己烷进一步脱脂。采用 HSS T3 C18 反相柱，以氨化甲酸缓冲液-乙腈梯度洗脱，用 MS/MS 检测，多反应监测，对氟喹诺酮残留进行 UPLC 分析。三文鱼组织中 DANO 的平均回收率为 73%，SARA 的回收率为 95%；虾中 DANO 的回收率为 71%，SARA 的回收率为 109%；罗非鱼中 DANO 的回收率为 62%，SARA 的回收率为 111%，回收率均在 1.0 ng g(-1)添加水平下。所有化合物的标准曲线在 0.002-0.5 ng 进样范围内均呈线性。CIPRO、DANO、ENRO 和 SARA 的检测限均为 0.2 ng g(-1)。对添加样品的操作误差、干扰和回收率表明，该方法适用于监管计划中的常规使用。推荐的方法简单、快速、特异、可靠，适用于三文鱼、罗非鱼和虾等水生动物中氟喹诺酮类药物残留的常规监测。
