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  • Title: Liquid chromatography coupled to quadrupole-Orbitrap high resolution mass spectrometry based method for target analysis and suspect screening of non-ionic surfactants in textiles.
    Author: Luo X, Zhang L, Niu Z, Ye X, Tang Z, Xia S.
    Journal: J Chromatogr A; 2017 Dec 29; 1530():80-89. PubMed ID: 29153579.
    Abstract:
    In this study, we describe a high-throughput and sensitive method for textiles analysis, using liquid chromatography coupled to quadrupole-Orbitrap high resolution mass spectrometry (LC-Q-Orbitrap HRMS), for the simultaneously quantitative analysis of 40 target alkylphenol polyethoxylates (APEO) oligomers with reference standards and screening of 160 alcohol polyethoxylates (AEO) oligomers without standards in textiles. The APEOs contain nonylphenol ethoxylates (NPEOs) and octylphenol ethoxylates (OPEOs) with an EO number of ethylene oxide of 1-20, while AEOs focus on C11EOs-C18EOs with an EO number of 1-20. After ultrasonic extraction in methanol, the extract was directly separated using a core-shell CORTECS C18+ column and analyzed by Full MS/dd-MS2 (data dependent acquisition) scan in ESI positive mode. Two best sensitivity experimental conditions for APEOs with short EO chains (AP(EO)1-2) and long EO chains (AP(EO)3-20) were investigated, respectively. Most APEO oligomers had wide concentration ranges and the correlation coefficients (R2) were higher than 0.999. The limit of quantitation (LOQ) values for NP(EO)3-20 oligomers ranges from 16.00 to 52.80μg/kg and for OP(EO)3-20 oligomers is from 2.40 to 8.00μg/kg. LOQ for NP(EO)1 and NP(EO)2, OP(EO)1 and OP(EO)2 was 2.40mg/kg and 0.24mg/kg, 1.20mg/kg and 0.16mg/kg, respectively. The average recovery for each APEO oligomer in cotton and polyester matrix was between 78% and 110% at three spiked levels and the relative standard deviation (RSD%) was below 10%. As to AEOs suspects, a HRMS compound database containing 160 AEO oligomers was built and several parameters such as exact m/z, isotopic patterns, predicted product ions and predicted retention time were used for screening and confirmation. The established method was successfully applied for analysis of 40 commercial textile samples. Compared with OPEOs, NPEOs, especially NP(EO)3-15 oligomers, were widely detected in samples and the total concentration ranged from 1.56 to 1376.31mg/kg. AEOs were also found in most samples, among which C12-14, C16 and C18 compounds appeared more frequently and the EO chains mainly ranged from 3 to 15.
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