| The degradation product of the non-ionic surfactant alkylphenol polyoxyethylene ether (APEO) - alkylphenol (AP) is a kind of environmental endocrine disruptors (EEDs), which has a significant effect of estrogen. And perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) is a class of persistent organic pollutants (POPs). These two substances have been prohibited by the EU to use in 1 textiles, leather or textile auxiliaries for import or export. In China, no relevant testing standards for these two kinds of materials have yet been published. So to develop a corresponding set of national standards and testing methods as soon as possible is an urgent need,and to carry out research in related fields will have positive effects and great significance on helping China to deal with the EU Technical Barriers on APs and PFOS.In this paper, ultrasonic extraction, solid-phase extraction pre-treatment method, combined with GC/MS methods were used to establish an effective method to detect alkylphenols (NP, OP) content in textile and textile auxiliaries. Textile samples were extracted with CH2C12 solution for the ultrasonic extraction, derivatization, the quantity of 4 -NP and 4-n-OP were determined using GC-MS-SIM quantitative analysis method. The pre-treatment conditions, derivatization conditions, chromatographic conditions,and ion selection were optimized. The recovery rate of this method was 80.73%～99.78%, with the relative standard deviation less than 5%. After solid-phase extraction, silylation derivatization, the auxiliaries samples were also determined using GC-MS-SIM quantitative analysis. For various kinds of auxiliaries, the pre-treatment methods were optimized through experiments. Recovery rate of various types of auxiliaries were above 90%, with the relative deviation less than 4% and the detection limit of 0.2mg/L. This method is applicable and can be extensively used for water, oil, emulsion and most of textile auxiliaries.In this paper, ultrasonic extraction and soxhlet extraction combined with UPLC -MS/MS analysis method were also used to establish the method to determine perfluorooctanoic acid and perfluorooctane sulfonate content in textile and leather. C18 column, 5mmol·L-1 ammonium acetate solution and acetonitrile gradient elution mixture, with flow rate of 0.2mL·min-1 was used. And triple quadrupole mass analyzer was used for qualitative and quantitative analysis. The detection limit was 1μg·L-1 the linear range (0～40.0μg·L-1) a linear relationship, and the correlation coefficients were all greater than 0.998. Textile samples by ultrasonic extraction of methanol 30min, at different concentrations of standard addition recovery rate of recovery of 78% or more, RSD is less than 7%. Leather samples used methanol as the solvent. After extraction by automatic Soxhlet extraction method, the samples were purified through composite weak anion-exchange column. The recovery rates were between 80% and 120%, with the relative standard deviation less than 15%, and the detection limit of 0.5mg·kg-1. The method is simple, convenient, and of high applicability.
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