Please use this identifier to cite or link to this item:
標題: Temperature controlled liquid phase microextraction in-situ derivatization for determination of estrogens in water by gas chromatography-tandem mass spectrometry
作者: 陳顗羽
Yi-Yu Chen
關鍵字: no
引用: 1. Quintana, J.B.; Carpinteiro, J.; Rodriguez, I.; Lorenzo, R. A.; Carro, A. M.; Cela, R., Determination of natural and synthetic estrogens in water by gas chromatography with mass spectrometric detection. J. Chromatogr. A 2004, 1024 (1-2), 177-185. 2. Zuo, Y.; Zhang, K.; Lin, Y., Microwave-accelerated derivatization for the simultaneous gas chromatographic-mass spectrometric analysis of natural and synthetic estrogenic steroids. J. Chromatogr. A 2007, 1148 (2), 211-8. 3. Liu, R.; Zhou, J. L.; Wilding, A., Microwave-assisted extraction followed by gas chromatography–mass spectrometry for the determination of endocrine disrupting chemicals in river sediments. J. Chromatogr. A 2004, 1038 (1-2), 19-26. 4. S. Streets, Endocrine Disrupting Compounds: A Report to the Minnesota Legislature,Minnesota Pollution Control Agency, 1998. 5. Tan, B. L.; Hawker, D. W.; Muller, J. F.; Tremblay, L. A.; Chapman, H. F., Stir bar sorptive extraction and trace analysis of selected endocrine disruptors in water, biosolids and sludge samples by thermal desorption with gas chromatography-mass spectrometry. Water res. 2008, 42 (1-2), 404-12. 6. Farke, C.; Rattenberger, E.; Roiger, S. U.; Meyer, H. H., Bovine colostrum: determination of naturally occurring steroid hormones by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS). J. Agric. Food Chem. 2011, 59, 1423-7. 7. Peng, X.; Wang, Z.; Yang, C.; Chen, F.; Mai, B., Simultaneous determination of endocrine-disrupting phenols and steroid estrogens in sediment by gas chromatography-mass spectrometry. J. Chromatogr. A 2006, 1116 (1-2), 51-6. 8. Noppe, H.; Verslycke, T.; De Wulf, E.; Verheyden, K.; Monteyne, E.; Van Caeter, P.; Janssen, C. R.; De brabander, H. F., Occurrence ofestrogens in the Scheldt estuary: a 2-year survey. Ecotoxicol. Environ. Saf. 2007, 66 (1), 1-8. 9. Alesha D. LaFleur, K. A. S., Determination of endocrine disruptors in water after derivatization with N-methyl-N-(tert.-butyldimethyl -trifluoroacetamide) using gas chromatography with mass spectrometric detection. J. Chromatogr. A 2000, 879(1), 97-112. 10.Labadie, P.; Budzinski, H., Determination of Steroidal Hormone Profiles along the Jalle d'Eysines River (near Bordeaux, France). Environ. Sci. Technol. 2005, 39 (14), 5113-5120. 11.Vanderford, B. J.; Pearson, R. A.; Rexing, D. J.; Snyder, S. A., Analysis of Endocrine Disruptors, Pharmaceuticals, and Personal Care Products in Water Using Liquid Chromatography/Tandem Mass Spectrometry. Anal. Chem. 2003, 75 (22), 6265-6274. 12.Tan, B. L.; Hawker, D. W.; Muller, J. F.; Tremblay, L. A.; Chapman, H. F., Stir bar sorptive extraction and trace analysis of selected endocrine disruptors in water, biosolids and sludge samples by thermal desorption with gas chromatography-mass spectrometry. Water res. 2008, 42 (1-2), 404-12. 13.Zhao, J. L.; Ying, G. G.; Wang, L.; Yang, J. F.; Yang, X. B.; Yang, L. H.; Li, X., Determination of phenolic endocrine disrupting chemicals and acidic pharmaceuticals in surface water of the Pearl Rivers in South China by gas chromatography-negative chemical ionization-mass spectrometry. Sci. Total Environ. 2009, 407 (2), 962-74. 14.LaFleur, A. D.; Schug, K. A., A review of separation methods for the determination of estrogens and plastics-derived estrogen mimics from aqueous systems. Anal. Chim. Acta 2011, 696(1), 6-26. 15.Harwood, D. T.; Handelsman, D. J., Development and validation of a sensitive liquid chromatography-tandem mass spectrometry assay to simultaneously measure androgens and estrogens in serum without derivatization. Clin. Chim. Acta 2009, 409(1-2), 78-84. 16.Kushnir, M. M.; Rockwood, A. L.; Bergquist, J.; Varshavsky, M.; Roberts, W. L.; Yue, B.; Bunker, A. M.; Meikle, A. W., High-sensitivity tandem mass spectrometry assay for serum estrone and estradiol. Am J Clin Pathol. 2008, 129, 530-9. 17.Tai, S. S. C.; Welsh, M. J., Development and evaluation of a reference measurement procedure for the determination of estradiol-17 beta in human serum using isotope-dilution liquid chromatography-tandem mass spectrometry. Anal. Chem. 2005, 77, 6359-6363. 18.Diaz-Cruz, M. S.; Lopez de Alda, M. J.; Lopez, R.; Barcelo, D., Determination of estrogens and progestogens by mass spectrometric techniques (GC/MS, LC/MS and LC/MS/MS). J. Mass Spectrom. : JMS 2003, 38 (9), 917-23. 19.Li, W.; Li, Y. H.; Li, A. C.; Zhou, S.; Naidong, W., Simultaneous determination of norethindrone and ethinyl estradiol in human plasma by high performance liquid chromatography with tandem mass spectrometry--experiences on developing a highly selective method using derivatization reagent for enhancing sensitivity. J. Chromatogr. B 2005, 825, 223-32. 20.Santa, T., ; Al-Dirbashi, O. Y ,; Fukushima,T., Derivatization reagents in liquid chromatography/electrospray ionization tandem mass spectrometry for biomedical analysis. Drug Discov Ther 2007, 2, 108-118. 21.Yamada, H.; Yamahara, A.; Yasuda, S.; Abe, M.; Oguri, K.; Fukushima, S.; Ikeda-Wada, S., Dansyl Chloride Derivatization of Methamphetamine: A Method with Advantages for Screening and Analysis of Methamphetamine in Urine. J. Anal. Toxicol. 2002, 26 (1), 17-22. 22.Fernández-González, V.; Concha-Graña, E.; Muniategui-Lorenzo, S.; López-Mahía, P.; Prada-Rodríguez, D., Solid-phase microextraction– gas chromatographic–tandem mass spectrometric analysis of polycyclic aromatic hydrocarbons: Towards the European Union water directive 2006/0129 EC. J. Chromatogr. A 2007, 1176 (1–2),48-56. 23.John Roboz, 'Mass spectrometry in cancer researchˮ, CRC Press,2002 24.Edmond de Hoffmann, Vincent Stroobant, 'Mass spectromrtry principles and applicationˮ , John Wiley & Sons, 2007 25.Dass, C. Fundament of contemporary mass spectrometry; John Wiley & Sons, 2007 26.李茂榮。「低能量碰撞誘導解離之串聯質譜儀」。質譜分析技術專 輯,民國 91 年,行政院國家科學委員會精密儀器發展中心編印, 頁 87-111 27.Pavlqvić D. M. Babić S. Horvat A. J.M. Kašelan-Macan, M., Sample preparation in analysis of pharmaceuticals. TrAC Trends in Anal. Chem. 2007, 26 (11), 1062-1075. 28. Pedersen- Bjergaard S. Rasmussen K. E. Liquid −Liquid −Liquid Microextraction for Sample Preparation of Biological Fluids Prior to Capillary Electrophoresis. Anal. Chem. 1999, 71 (14), 2650-2656. 29.Psillakis, E.; Kalogerakis, N., Developments in liquid-phase microextraction. TrAC Trends 2003, 22 (9), 565-574. 30.Ho, T. S.; Pedersen-Bjergaard, S.; Rasmussen, K. E., Recovery, enrichment and selectivity in liquid-phase microextraction: Comparison with conventional liquid–liquid extraction. J. Chromatogr. A 2002, 963 (1–2), 3-17. 31.Rasmussen, K. E.; Pedersen-Bjergaard, S., Developments in hollow fibre-based, liquid-phase microextraction. TrAC Trends 2004, 23 (1), 1-10. 32.Zhao, L. & Lee, H.K. Liquid-Phase Microextraction Combined with Hollow Fiber as a Sample Preparation Technique Prior to Gas Chromatography/Mass Spectrometry. Anal. Chem. 2002, 74, 2486-2492 33.Chao, Y.-Y.; Chien, T.-Y.; Kuo, T.-H.; Lu, Y.-A.; Shih, Y.-H.; Chen, S.-Y.; Hunag, Y.-L., On-line heat-assisted push/pull perfusion hollow fiber liquid–liquid–liquid microextraction for the rapid determination of phthalate esters in river water samples. Anal. Methods 2013, 5 (20), 5602. 34.Socas-Rodriguez, B.; Asensio-Ramos, M.; Hernandez-Borges, J.; Rodriguez-Delgado, M. A., Hollow-fiber liquid-phase microextraction for the determination of natural and synthetic estrogens in milk samples. J. Chromatogr. A 2013, 1313, 175-84. 35.Lee, M.-R.; Yeh, Y.-C.; Hsiang, W.-S.; Hwang, B.-H., Solid-phase microextraction and gas chromatography–mass spectrometry for determining chlorophenols from landfill leaches and soil. J. Chromatogr. A 1998, 806 (2), 317-324. 36.Liu, M.; Qiu, B.; Jin, X.; Zhang, L.; Chen, X.; Chen, G., Determination of estrogens in wastewater using three-phase hollow fiber-mediated liquid-phase microextraction followed by HPLC. Journal of separation science 2008, 31 (4), 622-8.
摘要: This study proposed a novel analytical method, temperature-controlled liquid phase microextraction in-situ derivatization combined with gas chromatography-tandem mass spectrometry for determination of trace estrogens in water samples. In optimum conditions, the octanol was utilized as extraction solvent and liquid membrane supported. An aliquot of 11.25 mL water sample (pH 6) containing 5% sodium chloride was mixed with 3.75 mL of 10 μg/mL dansyl chloride derivatization agent. After derivatization for 15 min at 60°C water bath, the derivatives was extracted by liquid phase microextraction with octanol then the extractant was analyzed by GC-MS/MS. The linearity of the proposed method ranged from 0.05 to 50 ng/mL and the coefficients of determination were above 0.9940. The limits of detection (LODs) of six estrogens studied were between 0.3 to 1.1 ng/mL. The intra-day and inter-day precisions ranged from 1.2 to 10.8% and 2.9 to 17.6%, respectively. The recovery of the presented method was between 84.9 and 107.8%. The results demonstrate the adequacy of the presented method for successful determination of trace estrogens in wastewater.
本研究開發以溫度控制液相微萃取 (liquid phase microextriction) 即時衍生化之前處理方式結合氣相層析串聯質譜術之分析,偵測水中六種微量雌激素化合物,包含雌酮、17α-雌二醇、17α-乙炔基雌脂二醇、美雌醇、二乙基己烯雌酚、雙烯雌酚。實驗結果顯示,在溫度控制液相微萃取即時衍生化前處理方法中,添加 5% 氯化鈉於水中,調整水樣為 pH6 和以 10 μg/mL 丹磺醯氯為衍生化試劑且以 3:1(v:v)的比例混合後置於 15 mL 樣品瓶中,將注滿 octanol 之中空纖維放入水樣中,在 60°C 水浴下,加熱衍生萃取 15 分鐘,再利用注射針取出中空纖維內之octanol直接以氣相層析串聯質譜儀進行分析。在最佳萃取與分析條件下分析水樣中六種雌激素之線性範圍介於 0.05 至 50 ng/mL 之間,線性相關係數皆在 0.9940 以上,方法偵測極限介於 0.3 至 1.1 pg/mL 之間。所開發分析方法之同日內精密度與異日內精密度相對標準偏差分別介於 1.2 至 10.8% 之間與 2.9 至 17.6% 之間, 回收率介於 84.9 至 107.8% 之間。應用所開發的方法於河川水、湖水、魚塭水、養豬廢水等各式廢水中微量雌激素之檢測,實驗結果顯示並未測出含有雌激素。本研究方法開發同時進行衍生化及萃取,不但可縮短樣品前處理時間且具高萃取效率以及選擇性,可做為水中微量雌激素之檢測參考。
文章公開時間: 10000-01-01
Appears in Collections:化學系所



Items in DSpace are protected by copyright, with all rights reserved, unless otherwise indicated.