纺织品中抗菌剂和紫外线吸收剂的同时测定

摘要

为监控纺织品中紫外线吸收剂和抗菌剂的含量,建立了同时测定纺织品中7种苯并三唑类紫外线吸收剂和7种抗菌剂含量的超高效液相色谱/静电场轨道阱高分辨质谱(UPLC/Orbitrap HRMS)方法.以甲醇为萃取溶剂,超声萃取纺织品中的苯并三唑类紫外线吸收剂和抗菌剂,萃取液经浓缩定容后进行UPLC/ Orbitrap HRMS分析,外标法定量.14种目标分析物的色谱分离在Hypersil GOLD色谱柱(100mm×2.1mm ×1.9μm)上进行,流动相为0.1%甲酸水溶液(含5mmol/L乙酸铵)/甲醇,三氯生和对氯间二甲酚(PCMX)采用电喷雾负离子模式,其余12种目标分析物采用电喷雾正离子模式,在m/z 100~m/z 500范围内进行一级质谱扫描.14种目标分析物的质量准确度误差均小于2×10-6,根据保留时间和准分子离子峰的精确质量数进行定性,根据提取离子色谱图的峰面积进行定量.对于每种目标分析物,在一定质量浓度范围内,提取离子色谱图峰面积均与其质量浓度线性相关,线性相关系数均大于0.998,检出限为0.1~0.3μg/kg.3个添加水平的平均回收率为80.9%~94.1%,相对标准偏差为3.6%~9.8%.采用该方法监测市售纺织品中紫外线吸收剂和抗菌剂的含量,结果在部分样品中检出不同含量水平的UV-327、三氯生、PCMX和2-正辛基-4-异噻唑啉-3-酮(OI).%In order to monitor the contents of antibacterial agents and ultraviolet absorbers in textiles, an effective method was established for the simultaneous determination of seven benzotriazole ultraviolet absorbers and antibacterial agents using ultra-high performance liquid chromatography/orbitrap high resolution mass spectrometry (UPLC/Orbitrap HRMS) technique.Fourteen target compounds were extracted with methanol and separated on a Hypersil GOLD column (100mm×2.1mm×1.9μm) with a gradient elution of methanol and 0.1% aqueous formic acid solution containing 0.5mmol/L ammonium acetate.Triclosan and 4-chloro-3,5-dimethyl phenol (PCMX) were detected by orbitrap HRMS in ESI negative mode while the other twelve target compounds were all detected by orbitrap HRMS in ESI positive mode.Full scan experiment was performed over the range from m/z 100 to m/z 500.Fourteen target compounds were routinely detected with the mass accuracy all below 2×10-6 (2ppm).The qualitative analysis was carried out by the retention time and the accurate mass of quasi-molecular ion and the quantitative analysis was carried out by the peak area in extracted chromatogram.Good linearities were achieved in the respective linear range for each target compound, with correlation coefficients higher than 0.998.The limits of detection (LODs) ranged from 0.1μg/kg to 0.3μg/kg.The blank samples were spiked at three levels and the spiked average recoveries varied from 80.9% to 94.1% while the relative standard deviation (RSD) changed from 3.6% to 9.8%.The method is simple, accurate and sensitive.