Aoyagi Mitsutoshi, Niiyama Kazuhito, Nemoto Satoru
Hokkaido Institute of Public Health, Sapporo.
Shokuhin Eiseigaku Zasshi. 2011;52(3):156-60. doi: 10.3358/shokueishi.52.156.
A method for the determination of clofencet in animal and fishery products was developed, using liquid chromatography with electrospray ionization mass spectrometry (LC/ESI-MS). The sample was homogenized with water and hexane, and the homogenate was extracted with acetonitrile, then acetonitrile-water (4 : 1). An aliquot of the crude extract was passed through a C18 cartridge column (1,000 mg), and the eluate was concentrated. A solution of 10% sodium chloride and 1% sodium hydrogen carbonate, and ethyl acetate were added to the residue, and the mixture was shaken. After shaking, the aqueous phase was recovered and acidified with hydrochloric acid, and then clofencet was extracted with ethyl acetate. The extract was evaporated to dryness and the residue was dissolved in methanol-water (3 : 7). Clofencet was analyzed by LC/MS. The recoveries of clofencet from ten kinds of animal and fishery products were 77.8-97.8%, and the relative standard deviations were 0.6-5.8% (n=5). S/N of the peak of clofencet was >10 and no interfering peak was found in animal and fishery products fortified at 0.01 mg/kg.
建立了一种采用液相色谱-电喷雾电离质谱联用仪(LC/ESI-MS)测定动物和水产品中氯苯乙腈的方法。样品用水和正己烷匀浆,匀浆液用乙腈萃取,然后用乙腈-水(4∶1)萃取。取部分粗提物通过C18柱(1000mg),洗脱液浓缩。向残渣中加入10%氯化钠和1%碳酸氢钠溶液以及乙酸乙酯,振摇混合液。振摇后,回收水相并用盐酸酸化,然后用乙酸乙酯萃取氯苯乙腈。萃取液蒸发至干,残渣溶于甲醇-水(3∶7)中。采用LC/MS分析氯苯乙腈。十种动物和水产品中氯苯乙腈的回收率为77.8%97.8%,相对标准偏差为0.6%5.8%(n=5)。氯苯乙腈峰的信噪比>10,在添加量为0.01mg/kg的动物和水产品中未发现干扰峰。