以密度比水小的溶剂为萃取剂,建立了涡旋辅助分散液液微萃取-气相色谱检测瓶装水中塑化剂的方法.传统分散液液微萃取技术一般采用密度大于水的有机溶剂为萃取剂.本方法以密度比水小的轻质溶剂正己烷-甲苯(1∶1,体积比)为萃取剂,乙腈为分散剂,涡旋辅助分散,离心后获得富集相,进行气相色谱检测,富集倍数高达171倍,具有良好的线性关系(相关系数为0.998 2~0.999 2)和精密度(3.1%~11.8%),以及较低的方法检出限(1.43~12.05 μg/L),加标回收率为81.2%~107.8%.该方法简便,快速,环保,可以用于测定实际水样中塑化剂.
A novel method of low-density solvent-based vortex-assisted dispersive liquid-liquid microextraction(DLLME)was developed for determination of plasticizer in bottled water by gas chromatography-flame ionization detection(GC-FID).Conventional DLLME methods usually employ organic solvents heavier than water as the extraction solvents.On the contrary, in this proposed extraction procedure, a mixture of low-density extraction solvent(toluene and n-hexane with V/V=1∶1)and dispersive solvent(acetonitrile)was injected into the aqueous sample solution to form an emulsion with vortex dispersed mode.The upper layer was collected and analyzed by GC after centrifugation.The enrichment factor was as high as 171.Under the optimized conditions, the proposed method provided a good linearity(R2=0.998 2~0.999 2)and the- DOI:10.3969/j.issn.1000-1565.2018.01.006基于轻质萃取剂的涡旋辅助分散液液微萃取-气相色谱法测定瓶装水中塑化剂张琪1,马瑶佳1,艾连峰2,吕运开1(1.河北大学 化学与环境科学学院,河北 保定 071002;2.河北出入境检验检疫局,河北 石家庄 050051)摘 要:以密度比水小的溶剂为萃取剂,建立了涡旋辅助分散液液微萃取-气相色谱检测瓶装水中塑化剂的方法.传统分散液液微萃取技术一般采用密度大于水的有机溶剂为萃取剂.本方法以密度比水小的轻质溶剂正己烷-甲苯(1∶1,体积比)为萃取剂,乙腈为分散剂,涡旋辅助分散,离心后获得富集相,进行气相色谱检测,富集倍数高达171倍,具有良好的线性关系(相关系数为0.998 2~0.999 2)和精密度(3.1%~11.8%),以及较低的方法检出限(1.43~12.05 μg/L),加标回收率为81.2%~107.8%.该方法简便,快速,环保,可以用于测定实际水样中塑化剂.关键词:气相色谱;涡旋辅助;分散液液微萃取;塑化剂;瓶装水中图分类号:O657.7 文献标志码:A 文章编号:1000-1565(2018)01-0033-08Determination of plasticizer in bottled water by low density solventbased vortex assisted dispersive liquid-liquid microextractioncombined with gas chromatographyZHANG Qi1, MA Yaojia1, AI Lianfeng2, Lü Yunkai1(1.College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China;2.Hebei Entry-Exit Inspection and Quarantine Bureau,Shijiazhuang 050051, China)Abstract: A novel method of low-density solvent-based vortex-assisted dispersive liquid-liquid microextraction(DLLME)was developed for determination of plasticizer in bottled water by gas chromatography-flame ionization detection(GC-FID).Conventional DLLME methods usually employ organic solvents heavier than water as the extraction solvents.On the contrary, in this proposed extraction procedure, a mixture of low-density extraction solvent(toluene and n-hexane with V/V=1∶1)and dispersive solvent(acetonitrile)was injected into the aqueous sample solution to form an emulsion with vortex dispersed mode.The upper layer was collected and analyzed by GC after centrifugation.The enrichment factor was as high as 171.Under the optimized conditions, the proposed method provided a good linearity(R2=0.998 2~0.999 2)and the- 收稿日期:2017-08-20 基金项目:国家自然科学基金资助项目(21375032);河北省自然科学基金资助项目(B2016201213) 第一作者:张琪(1992—),女,河北石家庄人,河北大学在读硕士研究生,从事食品安全分析研究.E-mail:zqsys1017@163.com 通信作者:吕运开(1967—),男,河北保定人,河北大学教授,博士,主要从事色谱分析与食品安全分析研究.E-mail:lvyunkai@hbu.edu.cn第1期张琪等:基于轻质萃取剂的涡旋辅助分散液液微萃取-气相色谱法测定瓶装水中塑化剂relative standard deviations(RSDs)were in the range of 3.1%~11.8%.The limits of detection(S/N=3)were in the range of 1.43~12.05 μg/L and the recoveries at three spiked levels were in the range of 81.2%~107.8%.It is a convenient, speedy, and environmentally benign for the routine analysis of plasticizer in water samples.
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