Research On High-resolution Mass Spectrometry Detection Technology For Prohibited And Restricted Substances In Ecological Textiles

This paper focuses on negative impact of prohibiting substances in ecological textile on human health and Chinese export trade.In view of the main problem in the detection of carcinogenic and allergenic dyes and phenolic compounds in textiles,taking ecological textiles as representative matrix,the rapid and high-throughput analysis techniques for arcinogenic and allergenic dyes and phenolic compounds is studied and mass spectrometric library of restricted compounds is established by using Orbitrap high-resolution mass spectrometry.Currently,mass spectrometric library of restricted compounds is mainly used by GC and low-resolution mass spectrometry.And High-resolution mass spectrometry is not involved in textiles,which caused high resolution mass spectrometry information of prohibited substances in textiles is insufficient.According to related international and domestic regulations,taking carcinogenic and allergenic dyes,phenolic compounds,pesticides,UV stabilizers,Flame retardant compounds and PFCs as main research objects,a screening database and mass spectrometric library of 129compounds were established.The established libraries contained 2622 mass spectra,131 MS spectra and 2491 MS² spectra,providing precursor and MS² fragments in HCD collision modes and giving optimal collision energy?CE?corresponding to MS²fragments.It provides accurate data for confirmation of related compounds in detection of textiles by high resolution mass spectrometry.A method for rapid screening and confirmation of harmful chemical dyes in textile is established by using Orbitrap high-resolution mass spectrometry.The dyes were extracted from textile samples with pyridine/water?1/1,v/v?under 95?,and filtered with 0.22?m membrane after diluted for HPLC-Quadrupole-Orbitrap analysis.Separating by C₁₈ chromatographic column and analyzing by Full MS/data dependence-MS² scan in positive/negative ESI mode.Harmful chemical dyes were simultaneously screened and confirmation by retention time,accurate mass of precursor ions,precursor ion isotopic pattern and accurate mass of product ions.The linear relationships for 47 dyes in the corresponding linear ranges are good,and the limits of quantitation were 0.01¹0 mg/kg.The recoveries of 47 dyes in cotton and polyester matrix were 62-120%with the relative standard deviations?RSDs?less than10%?n=6?.A method for rapid screening and confirmation of phenolic compounds in textile is established by using Orbitrap high-resolution mass spectrometry.The phenolic compounds were ultrasonic extracted from textile samples with methanol,added 0.1mL NaOH in the supernatant and blow-dry by N₂ under 40?.And dissolved by methanol/water?1/1,v/v?and filtered with 0.22?m membrane after diluted for HPLC-Q-Orbitrap analysis.Separating by Thermo Accucore aQ chromatographic column and analyzing by Full MS/dd-MS² data dependence scan in positive/negative ESI mode.Phenolic compounds were simultaneously screened and confirmation by retention time,accurate mass of precursor ions,precursor ion isotopic pattern and accurate mass of product ions.The linear relationships for 27 phenolic compounds in the corresponding linear ranges are good,and the limits of quantitation were 0.002⁵mg/kg.The recoveries of 27 phenolic compounds in cotton and polyester matrix were61%¹17%with the relative standard deviations?RSDs?less than 10%?n=6?.The main innovations of this study are:?1?a systemic high-resolution mass spectrometric screening library and high-resolution mass spectrometric library are established,to solve the problem of missing high-resolution mass spectrometric data and provide accurate data for confirmation of related compounds in detection of textiles by high resolution mass spectrometry.?2?A method for rapid screening and confirmation of 47 harmful chemical dyes and 27 phenolic compounds in textile is established by using Orbitrap high-resolution mass spectrometry.And using of pyrolysis inference software for fragmentation simulation to derive the composition of fragment ion and theoretical of fragment,which improved accuracy and reliability in identification of compounds.Compared with traditional methods,present work can the high-throughput detection,lower detection fees and shorten detection time.