Determination Of The PAEs In Textiles By In-Capillary SPE-GC-MS

Phthalate esters(PAEs)is a class of important environmental hormone,which is widely used in textile industry.PAEs can be through breathing,eating,and even skin contact into the human body and animal.After entering the organism,in addition to the general toxicity,it has the characteristics of carcinogenic,mutagenic and mutagenicity.The content of PAEs in textile countries established strict laws and regulations,and ordered that the PAEs limit in 0.1% weight ratio.So it is very necessary to analyze the PAEs in textiles.In order to solve the problems of complicated operation and low sensitivity in the detection of PAEs,a new sample pretreatment method which called in-capillary SPE method was been established,and the method was used for the detection and analysis of the combined with gas chromatography(GC)-mass spectrometry(MS),The research contents are as follows:(1)In this paper,the GC-MS analysis method of PAEs is established by selecting the column model,the sample inlet temperature,the heating procedure and the scanning mode.HP-5 capillary column was selected,and the sample inlet temperature was 250 ? as the optimum condition.The temperature was: 150 ?,hold 1.5 min;at 5? /min to 220 ?,hold1min;at 10 ? /min to 270 ?,hold 10 min.The scanning mode was selected by full scan and selective ion detection.(2)The extraction solvent and extraction time of PAEs were extracted from the textile,the different types of the solid phase extraction solvent,the amount of the elution agent,the sample rate and the elution rate were used to carry out the optimization of the solid phase extraction.The optimum extraction conditions were as follows: the textile samples were extracted with methanol by ultrasonic extraction 2 h;C18 as solid phase extraction column;5m L ethyl acetate elution,elution rate 3 m L/min.(3)A method for detecting PAEs in textiles by capillary SPE-GC-MS was established.Using C18 as filler in capillary-SPE column preparation and optimization of extraction conditions,and then it was combined with GC-MS qualitative and quantitative detection.In-capillary SPE optimal conditions were: 2 L methanol activation,loading velocity is 0.5 ?L/min,manual injection,thermal desorption,sample retention time is 4s.The experimental results show that the method of enrichment factor of PAEs is more than100 times and the linear relationship is good.The minimum detection limit of theinstrument is 0.21-0.53 ?g/L.The recovery rate of PAEs is 92.12%-109.0% and the relative standard deviation is less than 4%.The method is effective and convenient for the determination of trace amounts of phthalate esters in textiles.