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为了提高气相色谱-质谱法测定动物肌肉中己烯雌酚、双烯雌酚、己烷雌酚和双酚A残留时时样品的提取和净化效果,降低实验成本,建立了液液萃取的样品前处理方法,并对仪器测定方法进行了改进。选用DB-17MS毛细管柱,选择离子监测模式测定,双酚A-D16作内标物,内标法定量。4种检测物的检出限均能达到0.1μg/kg。在0.5,2.00,8.00μg/kg添加水平,回收率73.0%~119%,相对标准偏差(RSD)为3.5%~14%,检测物含量在1.0~80 ng/mL范围内,其含量与该化合物峰面积和内标物峰面积之比呈良好的线性相关,相关系数0.9992~0.9996。
In order to improve the extraction and purification effects of diethylstilbestrol, diethylstilbestrol, diethylstilbestrol and bisphenol A residues in animal muscle by gas chromatography-mass spectrometry and to reduce the experimental cost, a sample pretreatment method of liquid-liquid extraction was established. The method of measuring instruments has been improved. Selected DB-17MS capillary column, select the ion monitoring mode determination, bisphenol A-D16 as an internal standard, internal standard method. The detection limit of 4 kinds of test substances can reach 0.1μg / kg. The recoveries ranged from 73.0% to 119% with relative standard deviations (RSDs) of 3.5% to 14% at 0.5,2.00 and 8.00 μg / kg levels, and the contents of the analytes ranged from 1.0 to 80 ng / mL. Compound peak area and internal standard peak area ratio showed a good linear correlation, the correlation coefficient of 0.9992 ~ 0.9996.