Simultaneous Determination of Antibacterial Agents and Ultraviolet Stabilizers in Textiles by Ultra-high Performance Liquid Chromatography-Orbitrap High Re-solution Mass Spectrometry Coupled with Microwave-assisted Extraction

KeyWord:ultra-high performance liquid chromatography(UPLC)  orbitrap high resolution mass spectrometry(Orbitrap-HRMS)  4-chloro-3,5-dimethyl-phenol(PCMX)  ultraviolet stabilizers  isothiazolinone  triclosan  textiles  microwave-assisted extraction

Abstract:

      An effective method was established for the simultaneous determination of contents of seven antibacterial agents and seven ultraviolet stabilizers in textiles using ultra-high performance liquid chromatography-orbitrap high resolution mass spectrometric(UPLC/OrbitrapHRMS) technique.Antibacterial agents and ultraviolet stabilizers in textiles were microwave assistedly extracted at 85 ¡æ£¬using methanol as extraction solvent.Then the extract was concentrated,and analyzed by UPLC-Orbitrap HRMS with the external standard method.Fourteen target compounds were separated on a Hypersil GOLD column(100 mm¡Á2.1 mm£¬1.9 ¦Ìm) with a gradient elution of methanol and 0.1%aqueous formic acid solution consisting of 5 mmol/L ammonium acetate.Full scan experiment was performed in the range of m/z 100-500.Fourteen target compounds were routinely detected with the accuracy all below 2¡Á10-6(2 ppm).Among them£¬4-chloro-3,5-dimethyl phenol(PCMX) and triclosan were detected by orbitrap HRMS in ESI negative mode and the left twelve target compounds were all detected in ESI positive mode.The qualitative analysis was performed by the retention time and the accurate mass of quasi-molecular ion£¬while the quantitative analysis was performed by the peak area in extracted chromatogram.Good linearities were achieved in the respective linear ranges for each target compounds with their correlation coefficients all higher than 0.998.The spiked average recoveries ranged from 80.1%to 95.6%at three spiked levels while the relative standard deviation(RSD) varied from 2.9%to 10.5%.The limits of detection(LOD,S/N=3) changed from 0.1 ¦Ìg/kg to 0.3 ¦Ìg/kg.The proposed method was simple£¬accurate and sensitive£¬and could satisfy completely the demand for the determination of antibacterial agents and ultraviolet stabilizers in textiles.