气相色谱-质谱法测定鱼肉中8种环境激素的残留量

GC-MS Determination of of 8 Kinds of Environmental Endocrine Residues in Fish

提出了气相色谱-质谱法测定鱼肉中8种环境激素(辛基酚、壬基酚、双酚A、己烯雌酚、雌酮、17α-乙炔雌二醇、17β-雌二醇和雌三醇)含量的方法。样品经乙酸乙酯提取两次,过固相萃取柱净化后,将洗脱液氮吹至近干,再经七氟丁酸酐衍生后,氮吹至干,正己烷溶解。采用HP-5MS色谱柱分离,质谱测定中采用电子轰击离子源,选择离子监测模式。结果表明,方法检出限(3S/N)在0.1~0.3μg·kg^(-1),方法的回收率在71.64%~91.08%,测定值的相对标准偏差(n=6)为1.04%~3.20%。

GC-MS to determine the contents of 8 environmental endocrine(octyl phenol,nonyl phenol,bisphenol A,diethylstilbestrol,estrone,17α-ethinylestradiol,17β-estradiol and estriol)in fish.method.The sample was extracted twice with ethyl acetate,and after purification by a solid phase extraction column,the eluent was blown to near dryness with nitrogen,and then derivatized with heptafluorobutyric anhydride,the nitrogen was blown to dryness,and n-hexane was dissolved.The HP-5 MS chromatographic column is used for separation,the electron bombardment ion source is used in the mass spectrometry,and the ion monitoring mode is selected.The results show that the detection limit(3 S/N)of the method is 0.1~0.3μg·kg^(-1),the recovery rate of the method is 71.64%~91.08%,and the relative standard deviation of the measured value(n=6)is 1.04%~3.20%.