Determination Of Alkylphenol In Textiles By In-tube Capillary Solid-phase Extraction-gas Chromatography

Alkylphenols(APs) are synthetic raw materials and degradation products of thenon-ionic surfactant Alkylphenol polyethoxylates(APEOs). Octylphenol(OP) andnonylphenol(NP) are its representative substances, they widely exists in textiles astextile auxiliaries, in the use of textile process, OP and NP will into human body dueto perspiration, rubbing, washing and other reasons. OP and NP are kinds ofenvironmental estrogens, which have significant effects of endocrine disruptors on thehuman health, and have serious impacts. The contents of OP and NP have beenlimited in textiles, so to develop a rapid, simple and effective detection method of OPand NP will have positive effects.Due to the detection analyses of OP and NP belong to microscale even traceanalysis category, therefore, sample preparation is the key to ensure a successfulanalysis. Through the comparative study, we found that the previous pretreatmenttechnologies have many shortcomings, in order to avoid these disadvantages, thispaper puts forward a different mode of in-tube capillary solid-phase extractionpre-treatment method. The pretreatment method combined gas chromatographydetection, which is the the most widely used in alkylphenols detection, then, wedevelop a detection technology of in-tube capillary solid-phase extraction-gaschromatography, for the detection analyses of OP and NP in textiles.In this process of develop this new detection technology, at first, the capillaryextraction sorbents packing in the in-tube capillary were optimized. By comparing C18extraction column and Abselut NEXUS extraction column, we found that AbselutNEXUS column is better than C18column in the dosage of eluent, elution rate, sampletime, etc, and has the advantage of a significant breakthrough volume for OP and NP,so, in this experiment we choose the Abselut NEXUS sorbents to pack capillary.Determine the specifications and length of capillary, with the Abselut NEXUSsorbents packed. After the capillary is packed, we prepared a new in-tube capillary solid-phase extraction column. The target components were extracted and determinedin in-tube capillary solid-phase extraction optimization condition, use1.2μL methanoland1.2μL ultrapure water to activate the extraction column, sample velocity is0.7μL/min. Use the in-tube capillary solid-phase extraction coupled with gaschromatography, discussed the sample way, detection mode and thermal strippingtime. Eventually, we develop a method of in-tube capillary solid-phase extraction-gaschromatography. To optimized the experimental conditions of in-tube capillarysolid-phase extraction, we detect OP and NP by using the optimized in-tube capillarysolid-phase extraction-gas chromatography method, the detection limits of OP and NPwere4.7μg/L and5.2μg/L, respectively. We choose to added the OP and NP cottonfabrics textiles as the object of study, in the optimization of experimental conditions,the results showed that the recovery rate of OP was89%-100.5%, the recovery rateof NP was83%-98.5%. The relative standard deviation(RSD) were5.16%and6.08%,respectively. The results showed that this method can fast, simple and effective detectalkylphenols of textiles. Through the textile samples tested, we also proved thisextraction device has the advantages of simple manufacture, strong and durable, avariety selections of sorbents, high utilization rate, rather low volume of desorptionsolvent required and other characteristics. Advantages of the proposed methodincluded:simple, fast, no dead volume, excellent sensitivity and acceptablereproducibility.