微型基质固相分散GCECD法测定鲫鱼中18种有机氯农药残留

Micro Matrix Solid Phase Dispersion GC-ECD Procedure for Analysis of Organochlorine Pesticides in Crucian

建立了以LC-C18填料为分散剂,Alumina-N(中性氧化铝)为净化剂,乙腈为洗脱剂的微型基质固相分散法,并用气相色谱电子捕获检测器(GC-ECD)测定鲫鱼(Carassius auratus)肉中有机氯农药残留。对样品前处理及色谱条件的研究结果表明,在使用0.1 g样品、0.4 g LC-C18和0.1 g Alumina-N条件下,以2.5 mL乙腈的洗脱效果为较好,0.05、0.25和0.50 mg.kg-13个添加水平的回收率为73.0%～116.8%,相对标准偏差为1.6%～13.6%,所有组分检出限均在3.5μg.kg-1以下。

With the aid of GC-ECD （gas chromatography with electron capture detection）, a micro matrix solid phase dis- persion （MSPD） was used with LC-C18 as dispersant, Alumina-N as purificant and acetonitrile as eluting solvent to ana- lyze residues of organochlorine pesticides （OCPs） in the muscle of Carassius auratus. Results show that when 0. 1 g sam- pie, 0.4 g LC-C18 and 0. 1 g Alumina-N were used, the addition of 2. 5 mL aeetonitrile created a better elution effect with recovery rate varying in the range of 73.0% - 116. 8% for all the three sample spiking levels （0. 05, 0. 25 and 0. 50 mg ·kg^-1 ） and relative standard deviation in the range of 1.6% - 13.6%. The detection limits for all the fractions of or- ganochlorine stayed below 3.5 μg · kg^-1.