For Silk Products And Their Dyeing And Finishing Auxiliaries, Study On The Determination Of Ap And Apeo

Various dyes and additives are used in silk's chemical treatment process of dyeing and finishing. In this paper, owing to 2003/53/EC the new European Union restrictions on the production and use of APEO Act to APOE, the detection technology of n-octylphenol, nonylphenol, octylphenol ethoxylates and nonylphenol ethoxylates in the silk products was investigated, detection of APEO in silk products was established. The main content was concluded as follows:Using ultrasonic treatment and organic solvents to alkylphenolsor or alkyl polyoxyethylene was extracted in the silk sample pretreatment. The results show that for nonylphenol and octylphenol, the maximum effect of extraction is using dichloromethane to extract alkylphenols, nonylphenol ethoxylates for using methanol as the extraction of the most efficient. Using BSTFA+TMCS (99:1) as a derivatization reagent, the derivatization reaction is over at 90℃after 30min.According to the different additive form, the pretreatment of auxiliaries in silk samples, includes water-soluble and emulsion in liquid samples. deionized water as the medium was used for NP and OP simulation solution. For the target of analyte alkylphenol water-soluble additives, a certain volume ratio of methanol-methylene chloride eluant were selected. For the target of alkylphenol ethoxylates water-soluble additives, it can be directly dissolved by methanol. For their emulsion additive, sodium chloride and sodium sulfate must be added for demulsification. And then it can be determinated by solid phase extraction selecting the HR-X column for solid-phase column.For alkylphenols, according to external standard method of chromatographic peak area, it can definite the quantitative determination using selected ion on the basis of obtaining the retention time of isomers by GC-MS in full scan; for alkylphenol ethoxylates, NPnEO and OPnEO can be separated and determinated using bonded amino column as the stationary phase, water/acetonitrile as mobile phase gradient elution. The results show that the detection limit of octylphenol and nonylphenol is respectively 0.4mg/kg and 4mg/kg; the detection limit of alkylphenol ethoxylates is 10mg/kg fully reaching the testing requirement of alkylphenol ethoxylates residue in the textiles and textile auxiliaries.