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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 C 11 EOs-C 18 EOs with an EO number of 1-20. After ultrasonic extraction in methanol, the extract was directly separated using a core-shell CORTECS C 18 + column and analyzed by Full MS/dd-MS 2 (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 (R 2 ) 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 C 12-14 , C 16 and C 18 compounds appeared more frequently and the EO chains mainly ranged from 3 to 15., (Copyright © 2017. Published by Elsevier B.V.)

A comprehensive method for simultaneous identification and detection of 16 anabolic steroid hormones (ASs, including andorgens, gestagens and their esters) in muscle samples was developed with liquid chromatography coupled to quadrupole/linear ion trap mass spectrometry (LC-Q/Trap-MS). The ASs in muscle samples were extracted with acetonitrile under ultrasonic assistance. The extract was defatted by n-hexane with liquid-liquid partitioning and followed by clean-up with NH2 solid phase extraction (SPE) cartridge. The separation of analytes was carried out on a CAPCELL PAK C18 MG II column (150 mm x 2.0 mm, 5.0 microm) using mobile phases of 0.1% (v/v) formic acid in acetonitrile and 0.1% (v/v) formic acid-5 mmol/L ammonium formate aqueous solution with gradient elution. A scheduled multiple reaction monitoring (sMRM) in positive mode as survey scan and an enhanced product ion (EPI) scan as dependent scan in an information-dependent acquisition (IDA) experiment was adopted in mass spectrometry acquisition. On-line lab-built MS/MS library and internal standards were employed for the identification and quantification. As a result, the 16 ASs showed good linearity with all correlation coefficients (r) no less than 0. 999 0 within the linear ranges. The limits of quantification (LOQs, S/N > or = 10) for the 16 ASs were in the range of 0.029-0.36 microg/kg. At the three spiked levels (0.5, 2.0 and 20 microg/kg), the overall recoveries ranged from 89.9% to 118% with the relative standard deviations (RSDs) no more than 16.2% under within--laboratory reproducibility conditions. The proposed method can be used to identify and detect the 16 ASs in a single run, which makes it effective in residue surveillance of anabolic hormones in muscle samples.