超声萃取+GC/MS测定纺织品中的酚类抗菌剂

Determination of phenolic antibacterial agent in textiles with ultrasonic extraction+GC/MS

采用超声萃取和气质联用(GC/MS)分析技术,建立了抗菌纺织品中4-氯-3,5-二甲基苯酚(PCMX)和4-氯-3-甲基苯酚(PCMC)的测定方法。样品经甲醇超声萃取、浓缩后,用萃取剂定容,DB-5MS柱分离,选择离子(SIM)模式下定量检测。在优化的试验条件下,2种含氯酚的线性范围为0.1～100.0μg/mL,相关系数均大于0.999 1。定量下限分别为0.1 mg/kg和0.5 mg/kg,加标回收率为88.5%～92.6%,相对标准偏差均小于4.7%。该方法灵敏度高,操作简单,可用于抗菌纺织品中酚类化合物含量的快速检测。

Method for simultaneous determination of content of 4-chloro-3,5-dimethylphenol （PCMX） and 4-chloro-3-methylphenol （PCMC） in antibacterial textiles by gas chromatography-mass spectrometry（GC-MS） is established. Textiles are ultrasonically extracted with methanol as the extraction solvent. The extraction solution is concentrated and blown dry, and then redissolved in extraction solvent. The separation is carried out on an DB-SMS column. The separation of target compounds is performed with selected ion monitoring （SIM）. Under the optimal conditions, the calibration curves are linear in the range of 0. 1- 100 μg/mL, with correlation more than 0.999 1. The LOQ are 0.1 mg/kg and 0.5 mg/kg respectively. The spiked recoveries of two alkylphenols are between 88.5 % - 92.6% with the relative standard deviation （RSD） less than 4.7%. The proposed method is sensitive and rapid, and is suitable for the determination of PCMX and PCMC in antibacterial textiles.