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当前位置: 首页 > 文章 > 气相色谱-质谱法检测猪肌肉中8种性激素的残留 中国农业科学 2008 (9) 2776-2782
Position: Home > Articles > Multi-Residue Determination of Eight Anabolic Steroids by GC-MS in Muscle Tissues from Pig Scientia Agricultura Sinica 2008 (9) 2776-2782

气相色谱-质谱法检测猪肌肉中8种性激素的残留

作  者：
曾东平;林翠萍;曾振灵;黄显会;贺利民
单  位：
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
关键词：
性激素;GC-MS;多残留检测;猪肌肉
摘  要：
【目的】建立己烯雌酚、甲睾酮、炔诺酮、17α-乙炔雌二醇、雌二醇、6α-甲基-17α-羟基孕酮、苯甲酸雌二醇和乙酸氯地孕酮8种性激素在猪肌肉中残留的气相色谱-质谱(GC-MS)检测和确证方法。【方法】猪肌肉样品经过初提,去脂肪,固相萃取小柱净化,衍生化,最后用GC-MS检测和确证。【结果】此法在浓度2.5～50μg·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。
译  名：
Multi-Residue Determination of Eight Anabolic Steroids by GC-MS in Muscle Tissues from Pig
作  者：
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)
关键词：
Anabolic steroids; GC-MS; Multi-residue determination; Pigs
摘  要：
【Objective】A GC-MS method for 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 for diethylstilbestrol, 1.05, 3.50 μg·kg-1 for methyltestosterone, 1.19, 3.97 μg·kg-1 for norethindrone, 0.94, 3.13 μg·kg-1 for 17α-ethynylestradiol, 1.45, 4.83 μg·kg-1 for estradiol, 1.56, 5.20 μg·kg-1 for 6α-methyl-17α-hydroxy-progesterone, 1.92, 6.40 μg·kg-1 for estradiol benzoate, 2.41, 8.03 μg·kg-1 for chlormadinone acetate. 【Conclusion】These results showe that the method is widely available, accurate and sensitive.

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