气相色谱-串联质谱法测定生态纺织品中的邻苯二甲酸酯类
Determination of Phthalate Esters in Ecological Textile by GC-MS/MS
摘 要
采用气相色谱-串联质谱法同时测定生态纺织品中的24种邻苯二甲酸酯类。样品经正己烷超声提取,提取液经ProElut PSX玻璃固相萃取柱净化,以丙酮-正己烷(15+85)混合液洗脱,洗脱液经氮气吹至近干后,用正己烷定容至1.0 mL。采用DB-5MS毛细管色谱柱分离,质谱分析中采用电子轰击离子源和选择反应监测模式。24种邻苯二甲酸酯类的质量浓度在一定范围内与峰面积呈线性关系,检出限(3S/N)在1.0~10 mg·kg-1之间,测定下限(10S/N)在5.0~25 mg·kg-1之间。加标回收率在81.3%~102%之间,测定值的相对标准偏差(n=6)在1.8%~6.6%之间。
邻苯二甲酸酯类
生态纺织品
净化
GC-MS/MS
Phthalate esters
Ecological textile
Clean up
Abstract
GC-MS/MS was applied to the determination of 24 phthalate esters in ecological textiles. The sample was extracted with hexane. Then the extract was cleaned up by using ProElut PSX glass SPE column, with a mixture of acetone and hexane as eluant. The eluant was concentrated to dryness by N2 blowing and diluted to 1.0 mL with hexane. The analytes were separated on a DB-5MS capillary chromatographic column. EI and SRM were adopted in MS analysis. Linear relationships were found between the peak areas and the mass concentrations of 24 phthalate esters in definite ranges, with detection limits (3S/N) in the range of 1.0-10 mg·kg-1 and the lower limits of determination (10S/N) in the range of 5.0-25 mg·kg-1. Recovery rates obtained by standard addition method were in the range of 81.3%-102%, and RSDs (n=6) were in the range of 1.8%-6.6%.
中图分类号 DOI 10.11973/lhjy-hx201607013
所属栏目 工作简报
基金项目
收稿日期 2015/6/10
修改稿日期
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备注李爱军(1968-),男,吉林长春人,研究员,研究方向 为化学品、工业品、食品中有毒有害物质的检测。
引用该论文: LI Ai-jun,MOU Jun,ZHANG Dai-hui,HU Ting-ting,FU Yao,LIU Yang. Determination of Phthalate Esters in Ecological Textile by GC-MS/MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(7): 802～808
李爱军,牟 峻,张代辉,胡婷婷,付 瑶,刘 洋. 气相色谱-串联质谱法测定生态纺织品中的邻苯二甲酸酯类[J]. 理化检验－化学分册, 2016, 52(7): 802～808
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参考文献
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【2】BS EN 14372:2004 Child use and care articles - Cutleryand feeding utensils - Safety requirements and tests［S］．
【3】BS EN l5777:2009 Textiles - Test method for ph-thalates［S］．
【4】Test method: CPSC-CH-C1001-09.3 Standard operating procedure for determination of phthalates ［S］．
【5】GB/T 20388-2006 纺织品邻苯二甲酸酯的测定［S］．
【6】AIGNASSE M F, PROGNON P, STAEHOWICZ M, et al. Anewsim pleandra pid HPLC method for determination of DEHP in PVC paekaging and releasing studies［J］. Int J Phann, 1995,113(2):241-246．
【7】牛增元,叶曦文,房丽萍,等.固相萃取-气相色谱法测定纺织品中的邻苯二甲酸酷类环境激素［J］.色谱, 2006,24(5):503-507．
【8】王明泰,牟峻,靳颖.纺织品中邻苯二甲酸酯类增塑剂含量的测定［J］.印染, 2007(7):35-39．
【9】佟晓波,李莹.HPLC法测定化妆品中十六种邻苯二甲酸酯类化合物［J］.香料香精化妆品, 2012,6(3):33-38．
【10】卢佑演,湛社霞.HPLC法测定饮料中6种邻苯二甲酸酯类塑化剂的研究［J］.中国卫生检验杂志, 2013,23(11):2410-2416．
【11】白舟,李颢.荧光定量PCR法检测邻苯二甲酸酯的研究［J］.湖北农业科学, 2012,51(4):823-836．
【12】LIANG G, LEE H K. Vortex-assisted micro-solid-phase extraction followed by low-density solvent based dispersive liquid-liquid microextraction for the fast and efficient determination of phthalate esters in river water samples［J］. Journal of Chromatography A, 2013,1300:24-30．
【13】LIU H C, DEN W, CHAN S F, et al. Analysis of trace contamination of phthalate esters in ultrapure water using a modified solid-phase extraction procedure and automated thermal desorption-gas chromatography/mass spectrometry［J］. Journal of Chromatography A, 2008,1188(2):286-294．
【14】SUN M, DAI J N, WANG X F. Determination of phthalate esters in polyvinyl chloride infusion bag by stir bar sorptive extraction combined with GC［J］. J Sep Science, 2012,35(24):3486-3491．
【15】ZHOU X, SHAO X, SHU J J. Thermally stable ionic liquid-based sol-gel coating for ultrasonic extraction-solid-phase microextraction-gas chromatography determination of phthalate esters in agricultural plastic films［J］. Talanta, 2012,89:129-135．
【16】CHEN B, ZHANG L P. An easy and sensitive analytical method of determination of phthalate esters in children's toys by UPLC-MS/MS［J］. Polymer Testing, 2013,32(4):681-685．
【17】FENG Y L, ZHU J P, SENSENSTEIN R. Development of a headspace solid-phase microextraction method combined with gas chromatography mass spectrometry for the determination of phthalate esters in cow milk［J］. Analytica Chimica Acta, 2005,538(1):41-48．
【18】王明林,寇立娟,张玉倩,等.基质固相分散-气相色谱/质谱法测定蔬菜中的邻苯二甲酸酷［J］.色谱, 2007,25(4):577-580．
【19】KOLARIK B, BORNEHAG C, NAYDENOV K, et al. The concentration of phthalates in settled dust in Bulgarian homes in relation to building characteristic and cleaning habits in the family［J］. Atmospheric Environment, 2008,42(37):8553-8559．
【20】王成云,林君峰,岑杨媚,等.皮革制品中邻苯二甲酸酯类增塑剂含量的检测方法研究［J］.皮革科学与工程, 2013,3(2):20-24．
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