固相微萃取技术分析纺织品中全氟化合物
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摘要
采用二甲基十八烷基[3-三甲氧基硅丙基]氯化铵与纤维素基底表面的羟基发生硅烷化反应,制备出带有季铵盐(R_4N~+)正离子的新型固相微萃取涂层,采用扫描电子显微镜(SEM)和红外光谱(IR)表征涂层结构。将新型涂层用于纺织品中全氟化合物(OEKO-TEX Standard100中规定的9种)的分析,优化了影响涂层萃取效率的各个因素,建立了固相微萃取-液相二级质谱联用测试9种全氟化合物的方法。实验结果表明,方法线性相关系数R~2≥0. 9907,对于同一SPME萃取针精密度相对标准偏差(RSD)在4. 1%～9. 2%,不同萃取针精密度RSD在2. 6%～7. 9%,平均加标回收率为96. 3%～105. 9%,回收率相对标准偏差为2. 8%～11%。
A new type of solid phase microextraction( SPME) coating based on quaternary ammonium salt(R_4N~+) positive ion was prepared by silanization reaction of n-octadecyldimethyl[3-( trimethoxysilyl) propyl] ammonium chloride with hydroxyl groups on the surface of cellulose substrate. The SPME coating was characterized by scanning electron microscope( SEM) and infrared spectroscopy( IR). The factors that affect the extraction efficiency of the coating were optimized and a solid-phase microextraction-liquid chromatography-mass/mass spectrometry( MS/MS) method was established. The new coating was applied to analyze the perfluorinated compounds in textiles( 9 kinds specified in OEKO-TEX Standard 100). The experimental results showed that the method exhibited a good linearity with coefficients R~2≥0. 9907. The relative standard deviations( RSD) of precision were4. 1%-9. 2% for the same SPME probe and 2. 6%-7. 9% for different SPME probes. The extraction recoveries varied from 96. 3% to 105. 9% with RSDs of 2. 8%-11%. Compared with the method of GB/T 31126-2014,this method is easy to operate,highly selective and organic solvents-free.
A new type of solid phase microextraction( SPME) coating based on quaternary ammonium salt(R_4N~+) positive ion was prepared by silanization reaction of n-octadecyldimethyl[3-( trimethoxysilyl) propyl] ammonium chloride with hydroxyl groups on the surface of cellulose substrate. The SPME coating was characterized by scanning electron microscope( SEM) and infrared spectroscopy( IR). The factors that affect the extraction efficiency of the coating were optimized and a solid-phase microextraction-liquid chromatography-mass/mass spectrometry( MS/MS) method was established. The new coating was applied to analyze the perfluorinated compounds in textiles( 9 kinds specified in OEKO-TEX Standard 100). The experimental results showed that the method exhibited a good linearity with coefficients R~2≥0. 9907. The relative standard deviations( RSD) of precision were4. 1%-9. 2% for the same SPME probe and 2. 6%-7. 9% for different SPME probes. The extraction recoveries varied from 96. 3% to 105. 9% with RSDs of 2. 8%-11%. Compared with the method of GB/T 31126-2014,this method is easy to operate,highly selective and organic solvents-free.
引文
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[18] GB/T 31126-2014 Textiles—Determination of perfluorooctanesulfonates and perfluoroalkyl carboxylates GB/T 31126-2014纺织品全氟辛烷磺酰基化合物和全氟羧酸的测定
[2] Guo R,Cai Y Q,Jiang G B,Lam K S P. Prog. Chem.,2006,18(6):808
[3] Yang L,Li J G. Environ. Chem.,2015,34(4):649杨琳,李敬光.环境化学,2015,34(4):649
[4] Luo J,Zhu Y X,Liao Y,Hu J C. Chin. Fiber Insp.,2018,(1):74罗峻,朱奕轩,廖芸,胡剑灿.中国纤检,2018,(1):74
[5] OEKO-TEX Standard 100(2016)
[6] Belardi R P,Pawliszyn J B. Water Qual. Res. J. Can.,1989,24(1):179
[7] Li J Y,Wu Y H,Li H Y,Liu L Y,Wang Y,Yu Z. Shandong Chem. Ind.,2016,45(1):43李佳钰,吴雨杭,李昊原,刘丽艳,王莹,于湛.山东化工,2016,45(1):43
[8] Yuan B,Li F,Xu D,Fu M. Anal. Meth,2013,5(7):1739
[9] Gao F Q,Huang K J,Li H S,Liu X F,Lin C W. Chin. J. Anal. Lab.,2014,33(5):604高凡钦,黄克建,李宏森,刘晓峰,林翠梧.分析试验室,2014,33(5):604
[10] Chen Y,Xu X Y,Wang C,Lv Y B. Chinese J. Anal. Chem.,2015,43(7):1009陈烨,许秀艳,王超,吕怡兵.分析化学,2015,43(7):1009
[11] Wu L B,Chen C F,Zhang Q,Zeng Y. Guangzhou Chem.,2017,42(1):58伍利兵,陈朝方,张琼,曾煜.广州化学,2017,42(1):58
[12] Yang Y,Zhang C M,Liu N,Yao L,Chen C. Chin. Fiber Insp.,2016,(02):78杨杨,张成敏,刘娜,姚琳,陈晨.中国纤检,2016,(02):78
[13] Xu H,Tong H. J. Instrum. Anal.,2000,19(1):76许泓,佟晖.分析测试学报,2000,19(1):76
[14] Liu Y,Liang Y,Deng Z G,Song Y P. Dye.&Fin.,2005,31(18):37刘瑛,梁勇,邓志光,宋艳平.印染,2005,31(18):37
[15] Chen J,Zhang Y. Dye.&Fin.,2006,32(1):39陈军,张燕.印染,2006,32(1):39
[16] Deng J,Yang Y,Fang L,Lin L,Zhou H,Luan T. Anal. Chem.,2014,86(22):11159.
[17] Zhou C,Zhang X Y,Dai J B,Zhang H P. Chinese J. Chem. Phys.,2005,18(3):448周成,张兴元,戴家兵,张和平.化学物理学报,2005,18(3):448
[18] GB/T 31126-2014 Textiles—Determination of perfluorooctanesulfonates and perfluoroalkyl carboxylates GB/T 31126-2014纺织品全氟辛烷磺酰基化合物和全氟羧酸的测定