摘要
建立了气相色谱-质谱联用法测定纺织品中2-正辛基-4-异噻唑啉-3-酮(OIT)、4-氯-3-甲基苯酚(PCMC),2,4,6-三溴苯酚(2,4,6-TBP),2,6-二甲基苯酚(2,6-DMP)、对苯基苯酚(PPP)等5种防腐剂的方法。样品采用甲醇超声提取,提取液浓缩定容后,经DB-5MS石英毛细管柱分离,进行气相色谱-质谱联用仪分析,全扫描定性,选择离子定量。OIT、2,4,6-TBP、2,6-DMP的线性范围为0.3~20μg/m L,r≥0.9991,检出限为0.3 mg/kg;PCMC,PPP的线性范围为0.15~10μg/m L,r≥0.9993,检出限为0.15 mg/kg。5种防腐剂的回收率为72.7%~110%,RSD≤8.4%(n=6)。
A GC-MS method was developed for the determination of 5 preservatives,2-n-octyl-4-isothiazolin-3-one( OIT),4-chloro-3-methylphenol( PCMC),2,4,6-tribromophenol( 2,4,6-TBP),2,6-dimethylphenol( 2,6-DMP) and p-phenylphenol( PPP) in textiles. The sample was extracted with methanol in ultrasonic bath. The extract was concentrated and then volumed with methanol. The targets were separated on a DB-5MS quartz capillary column and full scan for qualitative analysis and selection scan for quantitative analysis by GC / MS. The calibration curves showed good linear relationship in the range of 0. 3 ~ 20 μg / m L for OIT,2,4,6-TBP,2,6-DMP and 0. 15 ~ 10 μg / m L for PCMC and PPP. The correlation coefficients were more than 0. 9991 for OIT,2,4,6-TBP,2,6-DMP and more than 0. 9993 for PCMC and PPP. The detection limits were 0. 3 mg / kg for OIT,2,4,6-TBP,2,6-DMP and 0. 15 mg / kg for PCMC and PPP. The recoveries ranged from 72. 7% to 110% with relative standard deviations lower than 8. 4%( n = 6).
出处
《分析试验室》
CAS
CSCD
北大核心
2015年第3期279-283,共5页
Chinese Journal of Analysis Laboratory
基金
福建检验检疫局科技计划项目(FK2012-38)资助