PMID- 23424876 OWN - NLM STAT- MEDLINE DCOM- 20131219 LR - 20130221 IS - 1000-8020 (Print) IS - 1000-8020 (Linking) VI - 41 IP - 6 DP - 2012 Nov TI - [Simultaneous determination of nine estrogens in eel by ultrafast liquid chromatography-tandem mass spectrometry with isotope dilution technique and solid-phase extraction]. PG - 956-62 AB - OBJECTIVE: Developing a rapid and sensitive analytical method based on ultrafast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) with solid-phase extraction (SPE) for the simultaneous determination of nine estrogens (dienestrol, diethylstilbestrol, estrone, hexestrol, 17-alpha-estradiol, 17-beta-estradiol, estriol, 17alpha-ethinylestradiol and estradiol valerate) in eel. METHODS: After the sample was extracted by acetonitrile and cleaned by Waters Oasis HLB solid-phase extraction cartridge, the UFLC separation was performed on a Shim-pack XR-ODS II column (100 mm x 2.0 mm, 2.2 microm) with a linear gradient elution program of methanol solution containing 0.04% ammonia (v/v) and 0.04% ammonia aqueous solution (v/v) as the mobile phase. Electrospray ionization was applied and operated in the negative multiple reaction monitoring (MRM) mode. The quantitation was used by isotope internal standard dilution technique. RESULTS: The results showed that the limits of quantitation (LOQs, S/N(10) were in the range of 0.07-0.4 microg/kg, the calibration curves were in good linearities for the nine analytes in the range of 0.5-50.0 microg/L with the correlative coefficients (r2) more than 0.998, the recoveries were between 81.0% and 110.0% with the relative standard deviations (RSDs) of 1.92%-8.24%. Additional, the mass spectra characterization of the nine estrogens was discussed and the fragmentation pathways were speculated. CONCLUSION: The developed method is rapid, sensitive, specific and reproducible, and adapts not only to the simultaneous determination of the nine trace estrogens including the epimer of 17-alpha-estradiol and 17-beta-estradiol but also to the identified detection in other fish tissues. FAU - Chen, Xiaohong AU - Chen X AD - Ningbo Municipal Center for Disease Control and Prevention, Ningbo Key Laboratory of Poison Research and Control, Ningbo 315010, China. chenxhnb@163.com FAU - Yao, Shanshan AU - Yao S FAU - Li, Xiaoping AU - Li X FAU - Zhao, Yonggang AU - Zhao Y FAU - Jin, Micong AU - Jin M LA - chi PT - English Abstract PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - China TA - Wei Sheng Yan Jiu JT - Wei sheng yan jiu = Journal of hygiene research JID - 9426367 RN - 0 (Estrogens) RN - 2DI9HA706A (Estrone) RN - 731DCA35BT (Diethylstilbestrol) RN - RRW32X4U1F (Dienestrol) SB - IM MH - Animals MH - Chromatography, Liquid/*methods MH - Dienestrol/analysis MH - Diethylstilbestrol/analysis MH - *Eels MH - Estrogens/*analysis MH - Estrone/analysis MH - Fish Products/*analysis MH - Food Contamination/analysis MH - Radioisotope Dilution Technique MH - Solid Phase Extraction/methods MH - Tandem Mass Spectrometry/*methods EDAT- 2013/02/22 06:00 MHDA- 2013/12/20 06:00 CRDT- 2013/02/22 06:00 PHST- 2013/02/22 06:00 [entrez] PHST- 2013/02/22 06:00 [pubmed] PHST- 2013/12/20 06:00 [medline] PST - ppublish SO - Wei Sheng Yan Jiu. 2012 Nov;41(6):956-62.