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作 者:尚岩岩 张岩岩 曾慧 SHANG Yanyan;ZHANG Yanyan;ZENG Hui(National Recycle Nonferrous Metals Rubber&Plastic Materials Quality Supervision and Inspection Center (Anhui),Fuyang Institute of Product Quality Supervision and Inspection,Fuyang 236000,China)
机构地区:[1]国家再生有色金属橡塑材料质量监督检验中心(安徽)阜阳市产品质量监督检验所,安徽阜阳236000
出 处:《化学分析计量》2019年第1期19-22,共4页Chemical Analysis And Meterage
基 金:国家质检总局科技计划项目(2015QK166)
摘 要:建立了测定塑料中1-甲基-2-吡咯烷酮含量的高效液相色谱–串联质谱法。以丙酮为提取剂,于室温下用超声波提取样品中的1-甲基-2-吡咯烷酮,提取液于35℃旋蒸至干,经甲醇溶解后,过0.22μm有机系滤膜。采用Innovation^(TM) C_(18)色谱柱(15 cm×2.1 mm,3.0μm)进行分离,用电喷雾电离(ESI)源、正离子模式进行扫描,以多反应监测模式检测。在优化的实验条件下,1-甲基-2-吡咯烷酮的质量浓度在1~50 ng/mL范围内与色谱峰面积呈良好的线性关系,线性相关系数为0.999 8,方法检出限为0.18μg/kg,样品加标回收率为75.0%~93.7%,测定结果的相对标准偏差为1.2%~2.8%(n=6)。该方法样品处理简单、快速,适用于塑料中1-甲基-2-吡咯烷酮的日常检测。A method was developed for the determination of 1-methyl-2-pyrroli-dinone in plastic products by high performance liquid chromatography-tandem mass spectrometry.Samples were extracted by ultrasonic with acetone as the extractant at room temperature,and the extracts were dried at 35℃.The final extracts were redissolved in methanol and filtered with 0.22μm syringe filter.The prepared samples were separated on an Innovation^TM C18 column (15cm×2.1mm,3.0μm) and characterized by using an electrospray ionization(ESI) source in the positive ion multiple reaction monitoring mode.Under optimum experimental conditions,good linearity was obtained in the range of 1-50ng/mL for 1-methyl-2-pyrroli-dinone with the correlation coefficient of 0.999 8.The detection limit was 0.18μg/kg.The spiked recoveries were 75.0%-93.7% and the relative standard deviations were 1.2%-2.8%(n=6).The method is simple and rapid to prepare the sample,and it can be used for the routine analysis of 1-methyl-2-pyrrolidinone in plastic products.
关 键 词:液相色谱-串联质谱法 1-甲基-2吡咯烷酮 塑料制品
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