Cao Xiaoji, Kong Qiaoling, Cai Ruonan, Zhu Kundan, Ye Xuemin, Chen Jiaoyu, Mo Weimin, Wang Jianli
Research Center of Analysis and Measurement, Zhejiang University of Technology, Hangzhou, Zhejiang, P.R. China.
J Sep Sci. 2014 Dec;37(24):3677-83. doi: 10.1002/jssc.201400824. Epub 2014 Nov 21.
An ultrasound-assisted magnetic solid-phase extraction procedure with chloromethylated polystyrene-coated Fe3 O4 nanospheres as magnetic adsorbents has been developed to determine eight phthalate esters (bis(4-methyl-2-pentyl) phthalate, dipentyl phthalate, dihexyl phthalate, benzyl butyl phthalate, bis(2-butoxyethyl) phthalate, dicyclohexyl phthalate, di-n-octyl phthalate, and dinonyl phthalate) simultaneously in beverage samples, in combination with gas chromatography coupled to tandem mass spectrometry for the first time. Several factors related to magnetic solid-phase extraction efficiencies, such as amount of adsorbent, extracting time, ionic strength, and desorption conditions were investigated. The enrichment factors of the method for the eight analytes were over 2482. A good linearity was observed in the range of 10-500 ng/L for bis(2-butoxyethyl) phthalate and 2-500 ng/L for the other phthalate esters with correlation coefficients ranging from 0.9980 to 0.9998. The limits of detection and quantification for the eight phthalate esters were in the range of 0.20-2.90 and 0.67-9.67 ng/L, respectively. The mean recoveries at three spiked levels were 75.8-117.7%, the coefficients of variations were <11.6%. The proposed method was demonstrated to be a simple and efficient technique for the trace analysis of the phthalate esters in beverage samples.
已开发出一种以氯甲基化聚苯乙烯包覆的Fe3O4纳米球作为磁性吸附剂的超声辅助磁性固相萃取方法,首次结合气相色谱-串联质谱法同时测定饮料样品中的8种邻苯二甲酸酯(邻苯二甲酸二(4-甲基-2-戊基)酯、邻苯二甲酸二戊酯、邻苯二甲酸二己酯、邻苯二甲酸苄基丁酯、邻苯二甲酸二(2-丁氧基乙基)酯、邻苯二甲酸二环己酯、邻苯二甲酸二正辛酯和邻苯二甲酸二壬酯)。研究了与磁性固相萃取效率相关的几个因素,如吸附剂用量、萃取时间、离子强度和解吸条件。该方法对8种分析物的富集倍数均超过2482。邻苯二甲酸二(2-丁氧基乙基)酯在10-500 ng/L范围内,其他邻苯二甲酸酯在2-500 ng/L范围内呈现良好的线性,相关系数在0.9980至0.9998之间。8种邻苯二甲酸酯的检出限和定量限分别在0.20-2.90 ng/L和0.67-9.67 ng/L范围内。三个加标水平的平均回收率为75.8-117.7%,变异系数<11.6%。所提出的方法被证明是一种用于饮料样品中邻苯二甲酸酯痕量分析的简单有效的技术。