【摘要】 建立了快速、灵敏的液相色谱-电喷雾串联质谱测定水产品中醋酸甲羟孕酮的残留量的方法。样品用乙酸乙酯提取,提取液用氮气吹干,乙腈溶解,正己烷初步除脂后,中性氧化铝小柱净化,浓缩定容。以V(乙腈)∶V(0.1%甲酸)=70∶30的溶液为流动相,采用Symmetry Shield RP18柱分离,通过电喷雾-串联四极杆质谱仪以多反应监测(MRM)方式进行检测。该方法准确、稳定、灵敏度高,在0.1~20μg/kg的添加范围内,醋酸甲羟孕酮的回收率为92%~106%,变异系数为3%~7%,检出限为0.03μg/kg,定量检出限为0.1μg/kg。更多还原

【Abstract】 The method of determination of medroxyprogesterone acetate residue in aquatic product by liquid chromatography with electrospray ionisation tandem mass spectrometric detection is described.The compound was extracted with ethyl acetate and evaporated to dryness,dissolved with acetonitrile and defatted with n-hexane,followed purified with neutral alumina solid-phase extraction cartridges.Sample was chromatographed using an acetonitrile-0.1% formic acid(7:3,v/v) mobile phase on a Symmetry Shield RP18 column.Analyte determination was performed by ESI-MS-MS in the multiple reaction monitoring(MRM) mode.The method was accurate and reproducible,at a spiking level from 0.1 μg/kg to 20 μg/kg,recovery ranged from 92% to 106%,coefficient of variation ranged from 3% to 7%,the limit of detection was 0.03 μg/kg and the limit of quantitation was(0.1) μg/kg.更多还原