A gas chromatography-mass spectrometry(GC-MS)method to determine eight anabolic steroids(diethylstilbestrol,methyltestosterone,norethindrone,17α-ethynylestradiol,estradiol,6α-methyl-17α-hydroxy-progesterone,estradi...A gas chromatography-mass spectrometry(GC-MS)method to determine eight anabolic steroids(diethylstilbestrol,methyltestosterone,norethindrone,17α-ethynylestradiol,estradiol,6α-methyl-17α-hydroxy-progesterone,estradiol benzoate,and chlormadinone acetate)was developed.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.In the above method,the linear scope was 2.5-50μg 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,and 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 were 0.99 and 3.30μg kg^-1 for diethylstilbestrol,1.05 and 3.50μg kg^-1 for methyltestosterone,1.19 and 3.97μg kg^-1 for norethindrone,0.94 and 3.13μg kg^-1 for 17α-ethynylestradiol,1.45 and 4.83μg kg^-1 for estradiol,1.56 and 5.20μg kg^-1 for 6α-methyl-17α-hydroxy-progesterone,1.92 and 6.40μg kg^-1 for estradiol benzoate,and 2.41 and 8.03μg kg^-1 for chlormadinone acetate,respectively.These results showed that the method was widely available,accurate,and sensitive.展开更多
基金supposed by the Projects of Agricultural Standards for Veterinary Drug Residues,China
文摘A gas chromatography-mass spectrometry(GC-MS)method to determine eight anabolic steroids(diethylstilbestrol,methyltestosterone,norethindrone,17α-ethynylestradiol,estradiol,6α-methyl-17α-hydroxy-progesterone,estradiol benzoate,and chlormadinone acetate)was developed.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.In the above method,the linear scope was 2.5-50μg 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,and 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 were 0.99 and 3.30μg kg^-1 for diethylstilbestrol,1.05 and 3.50μg kg^-1 for methyltestosterone,1.19 and 3.97μg kg^-1 for norethindrone,0.94 and 3.13μg kg^-1 for 17α-ethynylestradiol,1.45 and 4.83μg kg^-1 for estradiol,1.56 and 5.20μg kg^-1 for 6α-methyl-17α-hydroxy-progesterone,1.92 and 6.40μg kg^-1 for estradiol benzoate,and 2.41 and 8.03μg kg^-1 for chlormadinone acetate,respectively.These results showed that the method was widely available,accurate,and sensitive.
