高效液相色谱法测定纺织品中氯甲酚类生物杀灭剂

Determination of chlorocresols biocides in textiles by HPLC

建立同时测定纺织品中4-氯-3-甲基苯酚、4-氯-3,5-二甲基苯酚、2-苄基-4-氯苯酚和4-氯-2-[(5-氯-2-羟苯基)甲基]苯酚4种氯甲酚类生物杀灭剂的方法。样品经甲醇超声提取后,用Agilent Eclipse XDB-C18反相色谱柱(5μm,4.6 mm×250 mm)进行分离,以乙酸铵-甲醇为流动相,梯度洗脱,采用二极管阵列检测器(DAD)进行检测。在优化的试验条件下,在0.5~20.0 mg/L范围内,4种氯甲酚类生物杀灭剂的质量浓度与其色谱峰面积呈良好的线性关系,相关系数(R2)均为0.999,方法的检出限(S/N=3)为0.34~0.73 mg/kg,定量限(S/N=10)为1.1~2.4 mg/kg。2.5 mg/kg、10.0 mg/kg、50.0 mg/kg三个水平加标回收率为84%~97%,相对标准偏差小于5%(n=6)。该方法简单、快速、准确,适用于纺织品中氯甲酚类生物杀灭剂的测定。

A method for simultaneous determination of four chlorocresols biocides in textiles,including 4-chlo⁃ro-3-methylphenol,4-chloro-3,5-dimethylphenol,2-benzyl-4-chlorophenol,and 4-chloro-2-[(5-chloro-2-hydroxyphenyl)methyl]phenol,is established.Samples are extracted by methanol under ultrasonic conditions and separated using an Agilent Eclipse XDB-C18 reversed-phase chromatographic column(5μm,4.6 mm×250 mm).The mobile phase consists of ammonium acetate-methanol with gradient elution,and detection is performed using a diode array detector(DAD).Under optimized experimental conditions,the four chlorocresols biocides exhibit a good linear relationship between their mass concentrations in the range of 0.5-20 mg/L and their chromatographic peak areas,with a correlation coefficient(R2)of 0.999.The detection limits(S/N=3)of the method range of 0.34-0.73 mg/kg,and the quantification limits(S/N=10)range of 1.1-2.4 mg/kg.The recovery rates at three spiked levels of 2.5 mg/kg,10.0 mg/kg,and 50.0 mg/kg are between 84%and 97%,with a relative standard deviation of less than 5%(n=6).This method is simple,rapid,and accurate,making it suitable for the determination of chlorocresols biocides in textiles.