HPLC Determination of 3 Kinds of Short Chain 4-(1,1,3,3-Tetramethylbutyl)phenol, Ethoxylated in Textiles
摘 要
样品经甲醇超声萃取2次,萃取液浓缩后用异丙醇定容,分析物在Dikama platisil silica硅胶柱(250 mm×4.6 mm,5.0 μm)上分离,以正己烷-异丙醇(85+15)混合液为流动相A、异丙醇-水(85+15)混合液为流动相B进行梯度洗脱。采用荧光检测器检测,激发波长为230 nm,发射波长为296 nm。3种对特辛基苯酚乙氧基化物的线性范围均为0.50~50 mg·L-1,检出限(3S/N)在0.30~0.40 mg·kg-1之间。加标回收率在94.4%~106%之间,测定值的相对标准偏差(n=6)小于6.0%。
Abstract
The sample was ultrasonically extracted twice with methanol. The extract was concentrated and then diluted with isopropanol. The analytes were seperated on a Dikama Platisil silica column (250 mm×4.6 mm, 5.0 μm), with N-hexane-isopropanol (85+15) as mobile phase A, isopropanol-water (85+15) as mobile phase B for gradient elution. Fluoresence detector was used with the excitation wavelength of 230 nm and the emission wavelength of 296 nm. Linearity ranges of the 3 kinds of 4-(1,1,3,3-tetramethylbutyl)phenol, ethoxylated were all 0.50-50 mg·L-1, with detection limits (3S/N) of 0.30-0.40 mg·kg-1. Recovery rates obtained by standard addition method were in the range of 94.4%-106% and RSDs (n=6) were less than 6.0%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201709003
所属栏目 试验与研究
基金项目 宁波出入境检验检疫局科技计划项目(甬K05-2015);浙江省分析测试科技计划项目(2014C37089);浙江理工大学开放式基金(2014KF08)
收稿日期 2016/8/20
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备注任清庆(1986-)女,山东泰安人,工程师,硕士,主要从事纺织品检测方法与研究工作
引用该论文: REN Qingqing,BAO Qibei,FU Kejie,WU Feng,QIAN Dan. HPLC Determination of 3 Kinds of Short Chain 4-(1,1,3,3-Tetramethylbutyl)phenol, Ethoxylated in Textiles[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(9): 1002~1008
任清庆,保琦蓓,傅科杰,吴丰,钱丹. 高效液相色谱法测定纺织品中3种短链对特辛基苯酚乙氧基化物[J]. 理化检验-化学分册, 2017, 53(9): 1002~1008
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参考文献
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【10】吴彦霖,余炎,袁海霞,等.185 nm紫外光下薄液层中4-t-辛基酚的降解动力学:持久性有机污染物论坛2010暨第二届持久性有机污染物全国学术研讨会论文集[C].[出版地不详]:[出版者不详], 2010:174-175.
【2】AHEL M, GIGER W, KOCH M. Behaviour of alkylphenol polyethoxylate surfactants in the aquatic environment-I. Occurrence and transformation in sewage treatment[J]. Water Research, 1994,28(5):1143-1152.
【3】MA H W, CHENG Y. Determination of free and ethoxylated alkylphenols in leather with gas chromatography-mass spectrometry[J]. Journal of Chromatography A, 2012,1217(50):7914-7920.
【4】VEGA-MORALES T, SOSA-FERRERA Z, SANTANA-RODRIGUEZ J J. Determination of alkylphenol polyethoxylates, bisphenol-A, 17α-ethynylestradiol and 17β-estradiol and its metabolites in sewage samples by SPE and LC/MS/MS[J]. Journal of Hazardous Materials, 2010,183(1/3):701-711.
【5】DATLA V M, BECK K, SHIM E.Reverse phase HPLC analysis of commercial surfactants used as melt additives[J]. Tenside, Surfactants, Detergents, 2010,47(3):142-150.
【6】VANHOENACKER G, SANDRA P. High temperature liquid chromatography and liquid chromatography-mass spectroscopy analysis of octyphenol ethoxylates on different stationary phases[J]. Journal of Chromatography A, 2005,1082(2):193-202.
【7】WANG C, MA Q, WANG X. Determination of alkylphenol ethoxylates in textiles by normal-phase liquid chromatography and reversed-phase liquid chromatography/electrospray mass spectrometry[J]. Journal of AOAC International, 2007,90(5):1411-1417.
【8】LOOS R, HANKE G, UMLAUF G, et al. LC-MS-MS analysis and occurrence of octyl-and nonylphenol, their ethoxylates and their carboxylates in Belgian and Italian textile industry, waste water treatment plant effluents and surface waters[J]. Chemosphere, 2007,66(4):690-699.
【9】MARTÍNEZ E, GANS O, WEBER H, et al. Analysis of nonylphenol polyethoxylates with 3 to 10 ethoxy units in water samples by normal-phase liquid chromatography with electrospray mass spectrometry detection[J]. Fresenius Environmental Bulletin, 2005,14(8):681-689.
【10】吴彦霖,余炎,袁海霞,等.185 nm紫外光下薄液层中4-t-辛基酚的降解动力学:持久性有机污染物论坛2010暨第二届持久性有机污染物全国学术研讨会论文集[C].[出版地不详]:[出版者不详], 2010:174-175.
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