A　kind　of　homemade　solid-phase　microextraction　fibre　coupled　with　gas　chromatography-mass　spectrometry　(GC-MS)　was　developed　for　trace　analysis　of　antiestrogens　(tamoxifen,　cis-　and　trans-clomiphene)　in　biological　matrices.　In　this　method,　derivatization　was　unnecessary　and　sample　solution　Could　be　injected　directly　after　very　simple　deproteinization　operation.　The　conditions　of　influencing　adsorption　of　the　solid-phase　microextraction　(SPME)　fibre　and　desorption　of　the　analytes　were　investigated　gated　in　details.　Matrix　effects　were　studied　in　different　background.　Under　optimum　conditions　the,　proposed　method　was　further　validated　by　spiking　analytes　into　rabbit　liver　solutions.　Linear　ranges　of　tamoxifen.　cis-　and　trans-clomiphene　were　0.02-2.56,　0.08-2.56　and　0.16-2.56　ng　mL(-1),　respectively.　The　limits　of　quantitation　were　in　the　range　of　0.02-0.16　ng　mL(-1).　The　intra-day　accuracy　was　ranged　96.2-106.2%　and　precision　were　in　the　range　of　5.1-8.7%.　The　extraction　recoveries　of　the　antiestrogens　in　rabbit　liver　solution　were　between　73.8%　and　113.1%,　and　R.S.D.s　were　from　3.6%　to　14.1%.　The　results　show　that　the　homemade　sol-gel　coating　is　Suitable　for　determination　of　trace　antiestrogens　in　complex　matrices.　The　proposed　approach　was　proved　to　be　rapid,　simple,　easy,　sensitive　and　reproducible　for　trace　analysis　of　antiestrogens　in　biological　matrices.　(C)　2008　Elsevier　B.V.　All　rights　reserved.