PMID- 24354001 OWN - NLM STAT- MEDLINE DCOM- 20140505 LR - 20191210 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1318 DP - 2013 Nov 29 TI - Stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet/inductively coupled plasma mass spectrometry for analysis of thyroxine in urine samples. PG - 49-57 AB - tIn this work, polyethyleneglycol (PEG)/hydroxyl polydimethylsiloxane (OH-PDMS)/gamma -mercaptopropyltrimethoxysilane (gamma -MPTS) coated stir bar was prepared by sol-gel process and its extraction performance for the extraction of amphoteric thyroxines (3,3',5,5'-tetraiodothyronin, T(4); 3,3',5-triiodothyronine, T(3); reversed-3,3',5-triiodothyronine, rT(3)) and their metabolite (3,5-diiodothyronine,T2) was studied. The preparation reproducibility of PEG/OH-PDMS/gamma -MPTS coated stir bar was investigated, and the relative standard deviations (RSDs) in the same batch and among different batches were 3.3-14.3% (n = 5) and 7.7-16.6% (n = 3), respectively. The prepared PEG/OH-PDMS/gamma -MPTS coated stir bar could be reused for more than 20 times. Based on this fact, a novel method of stir bar sorptive extraction (SBSE) combined with high performance liquid chromatography (HPLC)-ultraviolet (UV)and HPLC-inductively coupled plasma mass spectrometry (ICP-MS) for the analysis of target thyroxinesin human urine samples was developed. The influencing factors of SBSE, such as sample pH, extraction time, stirring rate, salt effect, desorption solution and desorption time, were studied in detail, and the analytical performance of the proposed method was evaluated under the optimized conditions. The enrichment factors (EFs) of the developed method for four target thyroxines were in the range of 14.9-70.4(theoretical enrichment factor was 100). The RSDs were ranging from 4.0% to 13.8% for SBSE-HPLC-UV (c = 25 mug/L, n = 6) and from 3.7% to 6.1% for SBSE-HPLC-ICP-MS (c = 0.5 mug/L, n = 5). The linear range obtained by SBSE-HPLC-UV was 2-500 mug/L for T(2)and 5-500 mug/L for rT3, T(3)and T(4), with correlation coefficients (r) ranging from 0.9957 to 0.9998, respectively, while the linear range obtained by SBSE-HPLC-ICP-MS was 0.05-500 mug/L for T(2) and rT(3), 0.10-200 mug/L for T(3) and 0.05-200 mug/L for T(4)with r ranging from 0.9979 to 0.9998, respectively. The limits of detection (LODs) for the target thyroxines were 0.60-2.20 mug/L for SBSE-HPLC-UV and 0.0071-0.0355 mug/L SBSE-HPLC-ICP-MS, respectively. The developed method was applied for the determination of target thyroxines in urine samples, and the recovery for the spiking samples obtained by SBSE-HPLC-UV was in the range of 81.6-137.6% for human urine,while the recovery for the spiking urine samples obtained by SBSE-HPLC-ICP-MS were in the range of 72.0-121.5%. FAU - Fan, Wenying AU - Fan W FAU - Mao, Xiangju AU - Mao X FAU - He, Man AU - He M FAU - Chen, Beibei AU - Chen B FAU - Hu, Bin AU - Hu B LA - eng PT - Evaluation Study PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - Q51BO43MG4 (Thyroxine) SB - IM MH - Adsorption MH - Adult MH - Chromatography, High Pressure Liquid/*methods MH - Female MH - Humans MH - Limit of Detection MH - Male MH - Mass Spectrometry/*methods MH - Molecular Structure MH - Solid Phase Extraction/instrumentation/*methods MH - Spectrophotometry, Ultraviolet MH - Thyroxine/chemistry/*isolation & purification/*urine EDAT- 2013/12/20 06:00 MHDA- 2014/05/06 06:00 CRDT- 2013/12/20 06:00 PHST- 2013/12/20 06:00 [entrez] PHST- 2013/12/20 06:00 [pubmed] PHST- 2014/05/06 06:00 [medline] AID - S0021-9673(13)01622-1 [pii] AID - 10.1016/j.chroma.2013.10.022 [doi] PST - ppublish SO - J Chromatogr A. 2013 Nov 29;1318:49-57. doi: 10.1016/j.chroma.2013.10.022.