摘要
建立了超声震荡提取、硅胶小柱净化、气相色谱-质谱法测定鞋底材料(聚氯乙烯、热塑性橡胶、橡胶、聚氨酯、热塑性聚氨酯、飞龙和乙烯-醋酸乙烯共聚物)样品中16种邻苯二甲酸酯的方法。比较了索氏萃取与超声萃取的提取效果。以及硅胶、氧化铝、硅胶-氧化铝混合小柱的净化效果,本实验选择的萃取及净化条件为:常温下用二氯甲烷超声提取目标物40min(功率180W),经硅胶小柱净化分离后,用25.0mL乙酸乙酯/正己烷混合液(8?2,v/v)淋洗,淋洗液用氮气吹扫浓缩后进行GC-MS法测定。该方法的标准加入回收率为61.3%(DMP)～85.5%(DIDP,DDcP),相对标准偏差为1.3%～9.6%(n=6,0.50mg/L),检出限为4.3(DBP)～30.0(DUP)μg/g(3σ)。
A method of gas chromatography-mass spectrometry（GC-MS） was developed for the determination of 16 phthalate acid esters （PAEs） in commonly used sole materials, such as polyvinyl chloride （PVC）, thermoplastic rubber （TPR）, rubber, polyurethane （PU）, phylon, thermoplastic urethane （TPU）, ethylenevinyl acetate （EVA）, etc. The analytes （16 PAEs） were extracted with dichloromethane from samples with ultrasonic technique for 40 min at room temperature, and then purified and separated by a silica solidphase-extraction column with 25mL ethyl acetate and hexane mixture （8：2, v/v ） as eluant. After concentrated by nitrogen sweeping, the eluate was determined by GC-MS. The recoveries for standard spiked samples were 61. 3% （DMP）-85. 5% （DIDP, DDcP）. The RSDs were 1. 3%-9. 6% （n=6, 0. 50 mg/L）, and the detection limits （3a） were 4.3μg/g （DBP）-30.0μg/g （DUP） .
出处
《分析仪器》
CAS
2009年第2期15-20,共6页
Analytical Instrumentation
基金
福建省自然科学基金重点项目(B0220001)
