Christodoulou Eleni A, Samanidou Victoria F
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece.
J Sep Sci. 2007 Oct;30(15):2421-9. doi: 10.1002/jssc.200700129.
A rapid and sensitive analytical method was developed for the residue analysis of ten quinolones (enoxacin (ENO), ofloxacin (OFL), norfloxacin (NOR), ciprofloxacin (CIP), danofloxacin (DAN), enrofloxacin (ENR), sarafloxacin (SAR), oxolinic acid (OXO), nalidixic acid (NAL), and flumequine (FLU)) in cow's milk. The analytes were extracted from milk by a deproteinization step followed by a simple SPE cleanup procedure using LiChrolut RP-18 Merck cartridges. Recoveries varied between 75 and 92%. HPLC separation was performed at 25 degrees C using an ODS-3 PerfectSil Target (250 x 4 mm(2)) 5 microm analytical column (MZ-Analysentechnik, Germany). The mobile phase consisted of a mixture of TFA 0.1%-CH(3)CN-CH(3)OH, delivered by a gradient program at the flow rate of 1.2 mL/min. Elution of the ten analytes and the internal standard (caffeine, 7.5 ng/microL) was completed within 27 min. Column effluent was monitored using a photodiode array detector, set at 275 and 255 nm. The developed method was validated according to the criteria of Commission Decision 2002/657/EC. The LODs of the specific method of quinolones' determination in milk varied between 1.5 and 6.8 ng/microL.
开发了一种快速灵敏的分析方法，用于牛奶中十种喹诺酮类药物（依诺沙星（ENO）、氧氟沙星（OFL）、诺氟沙星（NOR）、环丙沙星（CIP）、达氟沙星（DAN）、恩诺沙星（ENR）、沙拉沙星（SAR）、恶喹酸（OXO）、萘啶酸（NAL）和氟甲喹（FLU））的残留分析。通过脱蛋白步骤从牛奶中提取分析物，然后使用默克LiChrolut RP - 18柱进行简单的固相萃取净化程序。回收率在75%至92%之间。使用ODS - 3 PerfectSil Target（250×4 mm²）5μm分析柱（德国MZ - Analysentechnik公司）在25℃下进行高效液相色谱分离。流动相由0.1%三氟乙酸 - 乙腈 - 甲醇的混合物组成，通过梯度程序以1.2 mL/min的流速输送。十种分析物和内标（咖啡因，7.5 ng/μL）在27分钟内洗脱完毕。使用光电二极管阵列检测器在275和255 nm波长下监测柱流出物。所开发的方法根据欧盟委员会第2002/657/EC号决定的标准进行了验证。牛奶中喹诺酮类药物特定测定方法的检测限在1.5至6.8 ng/μL之间。
