GC-MS法测定猪肉中雌激素类药物残留量

目的建立测定猪肉中己烯雌酚(diethylstilbestrol)、雌二醇(estradiol)、炔雌醇(ethinylestradi-ol)、戊酸雌二醇(estradiol valerate)残留量的GC-MS法,为控制食源性动物食品的质量提供依据。方法样品经乙酸乙酯提取,HLB固相萃取小柱净化,70℃衍生后在EI源SIM模式下进样分析。结果己烯雌酚、雌二醇、炔雌醇含量在2.0~100.0μg.kg-1内线性关系良好,戊酸雌二醇含量在4.0~200.0μg.kg-1内线性关系良好。己烯雌酚、雌二醇、炔雌醇、戊酸雌二醇相关系数分别为0.998 4、0.999 2、0.998 8、0.991 7,平均回收率(n=6)为78.3%~82.5%(RSD为4.4%~9.6%)。结论该方法为测定猪肉中这4种雌激素类药物残留量提供了可靠依据。

Analysis of estrogen residues in pork by gas chromatographic-tandem mass spectrometry

Objective To develop and validate a rapid sensitive and specific method for quantitative analysis of estrogen residues (DES, diethylstilbestrol; E2, estradiol; EE2, ethinylestradiol; EV, estradiol valerate) in pork by gas chromatographic-tandem mass spectrometry, which can be applied to the study of estrogen residues in pork. Method The 4 kinds of components were extracted from homogenized samples with ethyl acetate in base followed by solid-phase extraction with HLB column and trimethylsilylation at 70 ℃ for 40 minutes, then the GC-MS method in selected ion monitoring mode (SIM) was used. Results A good linearity was achieved with the coefficient r² > 0.991 7(n =2). The average recovery of estrogens was more than 71.7% with RSD lower than 7.2% ( n = 6). Conclusions The method is sensitive, accurate, rapid, and suitable for the analysis estrogen residues in pork.