基于中性解吸-电喷雾萃取电离质谱(ND-EESI-MS)建立了无需样品预处理即可直接检测蜂蜜中四环素的方法.测定结果表明,加标蜂蜜四环素样品在20~1000 ng/m L浓度范围内线性关系良好(R2〉0.997),检出限为1.08 ng/m L;加标浓度为50,500和1000 ng/m L蜂蜜样品的回收率分别为94.26%,98.38%和103.00%,精密度(RSD)分别为3.28%,1.39%和1.12%.应用此方法对8种市售蜂蜜进行检测,发现2种蜂蜜中含有痕量的四环素,其余蜂蜜均未检出,而应用高效液相色法在这8种市售蜂蜜中均未检出四环素.本方法无需经过复杂的样品预处理,灵敏度高、精密度好、分析速度快且特异性强,能够承受蜂蜜中复杂基体的影响,是一种快速检测蜂蜜中四环素的方法.
A novel platform of neutral desorption-extractive electrospray ionization mass spectrometry( ND-EESI-MS) for direct and rapid detection oftetracycline( TC) in honey sample without any sample pretreatment wa constructed. The results showed that the limit of detection was 1. 08 ng/m L with a linear working range from20 to 1000 ng/m L( R2〉0. 997) toward TC in honey; the recoveries and relative standard deviations of TC from spiked samples,at three fortification levels( 50,500,1000 ng/m L),were 94. 26%,98. 38%,103. 00%and 3. 28%,1. 39%,1. 12%,respectively. Eight common commodity honey samples were detected by this method and the results reveal that 2 of them contain traces of TC,while TC is not found in the rest samples.HPLC was also applied for TC detection in the asme honey samples,and TC is not found. Therefore,this ND-EESI-MS method is sensitive,rapid and specific for quantitative analysis of TC in honey without any sample pretreatment.