气相色谱-质谱法检测猪肌肉中8种性激素的残留.docVIP

气相色谱－质谱法检测猪肌肉中8种性激素的残留 曾东平，林翠萍，曾振灵，黄显会，贺利民 （华南农业大学兽医学院广东省兽药研制与安全评价重点实验室，广州 51064·kg-1保持良好的线性，相关系数大于0.97，在2.5、10、50μg·kg-1的添加水平上，8种性激素各组分的回收率（%）、批内变异系数（%）、批间变异系数（%）的范围分别为：己烯雌酚78.5～148、6.3～12和8.9～10，甲睾酮70.8～109、4.1～11和6.6～7.5，炔诺酮69.8～87.2、4.0～10和6.7～8.8，17α-乙炔雌二醇67.7～120、4.2～12和9.3～10，雌二醇82.8～103、0.4～10和6.8～11，6α-甲基-17α-羟基孕酮70.3～99.2、2.7～9.3和5.9～7.8，苯甲酸雌二醇73.0～104、5.4～12和9.7～12，乙酸氯地孕酮72.9～91.8、3.3～9.2和8.0～8.6。检测限和定量限（μg·kg-1）分别为：己烯雌酚0.99和3.30；甲睾酮1.05和3.50；炔诺酮 1.19和3.97；17α-乙炔雌二醇0.94和3.13；雌二醇 1.45和4.83；6α-甲基-17α-羟基孕酮1.56和5.20；苯甲酸雌二醇 1.92和6.40；乙酸氯地孕酮2.41和8.03。【结论】所建立的检测方法具有简便、准确、灵敏、适用性强及有机溶剂污染小等特点。 关键词：性激素；GC-MS；多残留检测；猪肌肉 Multi-Residue Determination of Eight Anabolic Steroids by GC-MS in Muscle Tissues from Pig ZENG Dong-ping, LIN Cui-ping, ZENG Zhen-ling, HUANG Xian-hui, HE Li-min (Laboratory of Veterinary Pharmacology/ College of Veterinary Medicine, South China Agricultural University, Guangzhou 510640) Abstract: 【Objective】A GC-MS method determination of eight anabolic steroids (diethylstilbestrol, methyltestosterone, norethindrone, 17α-ethynylestradiol, estradiol, 6α-methyl-17α-hydroxy-progesterone, estradiol benzoate, chlormadinone acetate) was developed. 【Method】Muscle samples were extracted with liquid-liquid extraction and clean-up was performed in two steps, the extracts obtained were derivatized with heptafluorbutyric (HBF) anhydride and analyzed by GC-MS.【Result】In the above method, the linear scope was 2.5-50 (μg·kg-1). The range of the recoveries was 78.5%-148% for diethylstilbestrol, 70.8%-109% for methyltestosterone, 69.8%-87.2% for norethindrone, 67.7%-120% for 17α-ethynylestradiol, 82.8%-103% for estradiol, 70.3%-99.2% for 6α-methyl-17α-hydroxy-progesterone, 73.0%-104% for estradiol benzoate, 72.9%-91.8% for chlormadinone acetate. The range of the coefficients of variation within batches was 0.4%-12%; The range of the coefficients of variation between batches was 6.4%-11%. The limit of detections and the detection capability was 0.99, 3.30 μg·kg-1 fo