摘要
建立了测定纺织品中壬基酚聚氧乙烯醚和辛基酚聚氧乙烯醚的硅胶吸附色谱-电喷雾质谱分析方法。不同类型的纺织品样品采用加速溶剂萃取法,以无水乙醇为提取溶剂,在10.3MPa和100℃下静态循环提取2次,提取液经Sep-Pak Carbon/NH2石墨化碳黑/氨基复合型固相萃取柱净化,以Waters Spherisorb S3W(150mm×2.0mm,3μm)色谱柱为分离柱,乙腈-水体系为流动相梯度洗脱,在电喷雾质谱正离子模式下进行定性及定量分析。壬基酚聚氧乙烯醚的方法检出限为10～40μg/kg,在1～20mg/kg的3个添加水平范围内的平均回收率为81.4%～95.9%,相对标准偏差均小于12.5%。辛基酚聚氧乙烯醚的方法检出限为10～30μg/kg,在1～20mg/kg的3个添加水平范围内的平均回收率为80.2%～96.8%,相对标准偏差均小于13.0%。本方法准确、简便、快速,可用于纺织品的实际检验工作。
A comprehensive analytical method based on silica adsorption chromatography-electrospray mass spectrometry has been developed for the determination of nonylphenol ethoxylates and octylphenol ethoxylatesin textiles. Various textile samples were extracted under 10.3 MPa and 100 ℃ by accelerated solvent extraction method with two static cycles using ethanol as the extraction solvent. The extract was cleaned up by carbon/NH2 solid phase extraction cartridge. After the chromatographic separation on a Waters Spherisorb S3W（ 150 mm × 2.0 mm, 3 μm）column by acetonitrile-water gradient elution, qualitative and quantitative a- nalysis was carried out by ESI/MS in the positive ion mode. The limits of detection （LODs） for nonylphenol ethoxylates were in the range of 10 -40 μg/kg. The mean recoveries at the spiked level of 1 -20 mg/kg were 81.4% -95.9%, with the relative standard deviation less than 12.5%. The limits of detection （LODs） for octylphenol ethoxylates were in the range of 10 -30μg/kg. The mean recoveries at the spiked level of 1 -20 mg/kg were 80.2% -96.8% , with the relative standard deviation less than 13.0%. The method is accurate, simple, rapid and adapts to the inspection of alkylphenol ehthoxylates in textiles.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2009年第1期46-52,共7页
Chinese Journal of Analytical Chemistry
基金
国家质量监督检验检疫总局科技计划(No.2006IK080)资助项目
关键词
加速溶剂萃取
固相萃取
硅胶吸附色谱
电喷雾质谱
纺织品
烷基酚聚氧乙烯醚
Accelerated solvent extraction, solid phase extraction, silica adsorption chromatography, electrospray mass spectrometry, textiles, alkylphenol ethoxylates
