title: A method by homemade OH/TSO-PMHS fibre solid-phase microextraction coupling with gas chromatography-mass spectrometry for analysis of antiestrogens in biological matrices.
abstract: 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 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.
authors.affiliation: Ministry of Education Key Laboratory of Analysis and Detection for Food Safety (Fuzhou University), Analytical and Testing Center, The Sport Science Research Center, Fuzhou University, Fuzhou, Fujian 350002, China.
authors.forename: Wei
authors.initials: W
authors.lastname: Liu
authors.forename: Lan
authors.initials: L
authors.lastname: Zhang
authors.forename: Shengping
authors.initials: S
authors.lastname: Chen
authors.forename: Hongbin
authors.initials: H
authors.lastname: Duan
authors.forename: Xi
authors.initials: X
authors.lastname: Chen
authors.forename: Zhenyi
authors.initials: Z
authors.lastname: Wei
authors.forename: Guonan
authors.initials: G
authors.lastname: Chen
mesh_terms: D000327:Adsorption; D000818:Animals; D020847:Estrogen Receptor Modulators / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry; D006798:Housing; D006863:Hydrogen-Ion Concentration; D006878:Hydroxides / Q000737:chemistry*; D008099:Liver / Q000737:chemistry; D011817:Rabbits; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012827:Silicone Oils / Q000737:chemistry*; D012833:Siloxanes / Q000737:chemistry*; D012965:Sodium Chloride / Q000737:chemistry; D052617:Solid Phase Microextraction / Q000379:methods*; D013696:Temperature; D013997:Time Factors
chemical_list: D020847:Estrogen Receptor Modulators; D006878:Hydroxides; D012827:Silicone Oils; D012833:Siloxanes; C402373:poly(methylhydrosiloxane); D012965:Sodium Chloride; C031356:hydroxide ion