[Determination of hormone multi-residues in animal tissues by gas chromatography-mass spectrometry].
A method of gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of nine sex hormone residues, such as hexestrol, diethylstilbestrol, dienestrol, etiocholan-3alpha-ol-17-one, epitestosterone, estrone, estradiol, ethinylestradiol and estriol, in animal tissues was developed. The sex hormones were extracted with acetonitrile, then cleaned-up with a C18 solid-phase extraction (SPE) column. The microwave-assisted derivatization of the target components with N,O-bis( trimethylsilyl) trifluoroacetamide (BSTFA) and trimethylchlorosilane (TMCS) (99:1, v/v) using pyridine as solvent was performed, and then the derivatives were analyzed by GC-MS. The limits of detection were 0.1-1 microg/kg for all hormones, and the limits of quantification were 0.2-2 microg/kg. The average recoveries of sex hormones were 68.8%-93.1%. The relative standard deviations (RSDs) of inter- and intra-assay were 4.1%-22.3% and 3.1%-17.9%, respectively. The real sample tests showed this method can be used for the sensitive and accurate determination of multi-sex hormones residues in biological samples.
Liaoning Entry-Exit Inspection and Quarantine Bureau, Dalian 116001, China. dlciqlwx@sina.com.cn
Weixuan
W
Lin
Weifeng
W
Dong
Xi
X
Chen
Miao
M
Tian
Ling
L
Yu
Jinghong
J
Zhao
Chunguang
C
Yang
D000818:Animals; D004350:Drug Residues / Q000032:analysis*; D004845:Epitestosterone / Q000032:analysis; D004958:Estradiol / Q000032:analysis; D005506:Food Contamination / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D012739:Gonadal Steroid Hormones / Q000032:analysis*; D006589:Hexestrol / Q000032:analysis; D008461:Meat Products / Q000032:analysis*; D013552:Swine
D012739:Gonadal Steroid Hormones; D006589:Hexestrol; D004845:Epitestosterone; D004958:Estradiol