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色谱  2006 

Determination of Residues of Three Stilbene Drugs in Animal Tissues Using Gas Chromatography-Mass Spectrometry
气相色谱-质谱法测定动物组织中三种1,2-二苯乙烯类药物的残留量

Keywords: solid phase extraction(SPE),gas chromatography(GC),mass spectrometry(MS),stilbenes,residue,animal tissues
固相萃取
,气相色谱,质谱,1,2-二苯乙烯类药物,残留,动物组织

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Abstract:

A method has been developed to determine residual stilbenes such as diethylstilbestrol (DES), dienestrol (DIS) and hexestrol (HS) in animal tissues using solid phase extraction (SPE) and gas chromatography-mass spectrometry (GC-MS). The procedures for extraction, cleanup on an LC-Si solid phase extraction cartridge and derivatization of stilbenes were established and optimized. The analytes were detected by mass spectrometer with electron impact source in selected ion monitoring mode (EI/SIM), and quantified with an external standard calibration curve method. Linear calibration curves were obtained in the concentration ranges from 5 to 500 microg/L for HS and from 10 to 1000 microg/L for DES and DIS (the correlation coefficients were above 0.99). Recoveries of the stilbenes were 73.0%-86.5%, and the relative standard deviations were between 1.0% and 7.2%. The limits of detection were 0.30 microg/kg for cis-DES, 0.10 microg/kg for trans-DES and HS and 0.15 microg/kg for DIS in pork and swine liver.

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