Huang Jing-Fang, Zhang Hui-Juan, Feng Yu-Qi
Department of Chemistry, Wuhan University, Wuhan 430072, and Wuhan Institute for Drug Control, Wuhan, PR China.
J Agric Food Chem. 2006 Dec 13;54(25):9279-86. doi: 10.1021/jf062246e.
A rapid confirmatory method for monitoring chloramphenicol (CAP) residues in honey, whole milk, and eggs is presented. This method is based on the polymer monolith microextraction (PMME) technique and high-performance liquid chromatography (HPLC)-electrospray ionization mass spectrometry (MS). A poly(methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary column was selected as the extraction medium. To obtain optimum extraction efficiency, several parameters related to PMME were investigated. After dissolution in 20 mM phosphate solution at pH 4.0 and centrifugation, honey, eggs, or milk samples were directly passed through the extraction tube. The LC-MS instrument was equipped with an electrospray ion source and a single quadrupole. The eluates were analyzed by LC-MS in the negative-ion mode and by monitoring a pair of isotopic ions for the target compound. The in-source collision-induced dissociation process produced confirmatory ions. The recoveries of CAP from real samples spiked at 0.1-10 ng/g (honey), 0.2-10 ng/mL (milk), and 0.2-10 ng/g (egg) were in the range of 85-102%, with relative standard deviations ranging between 2.1% and 8.9%. The limits of detection (S/N = 3) were 0.02 ng/g, 0.04 ng/mL, and 0.04 ng/g in honey, milk, and eggs, respectively. The proposed method was proved to be robust in monitoring CAP residue in honey, milk, and eggs.
本文提出了一种用于监测蜂蜜、全脂牛奶和鸡蛋中氯霉素(CAP)残留的快速确证方法。该方法基于整体柱微萃取(PMME)技术和高效液相色谱(HPLC)-电喷雾电离质谱(MS)。选用聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯)整体柱毛细管作为萃取介质。为了获得最佳萃取效率,研究了与PMME相关的几个参数。蜂蜜、鸡蛋或牛奶样品在pH 4.0的20 mM磷酸盐溶液中溶解并离心后,直接通过萃取管。液相色谱-质谱联用仪配备电喷雾离子源和单四极杆。洗脱液通过液相色谱-质谱联用仪在负离子模式下进行分析,并通过监测目标化合物的一对同位素离子进行检测。源内碰撞诱导解离过程产生确证离子。在蜂蜜中添加0.1 - 10 ng/g、牛奶中添加0.2 - 10 ng/mL、鸡蛋中添加0.2 - 10 ng/g的CAP,实际样品的回收率在85% - 102%之间,相对标准偏差在2.1% - 8.9%之间。蜂蜜、牛奶和鸡蛋中的检测限(S/N = 3)分别为0.02 ng/g、0.04 ng/mL和0.04 ng/g。所提出的方法在监测蜂蜜、牛奶和鸡蛋中的CAP残留方面被证明是可靠的。