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全二维气相色谱-飞行时间质谱法测定塑料中50种高关注物质
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周龙龙,薛秋红,刘一龙,牛增元,罗忻,尹桂林,马强,谢堂堂 1.青岛海关技术中心2.中国检验检疫科学研究院3.深圳海关工业品检测技术中心 
基金项目:国家重点研发计划资助项目(2016YFF0203702);海关总署科研项目(2019HK070);青岛海关科研项目(QK202006)
中文摘要:该文建立了塑料制品中50种高关注物质(24种多环芳烃、17种邻苯二甲酸酯类塑化剂、3种烷基酚、4种苯并三唑类紫外稳定剂、1种卡拉花醛香料和1种磷酸三(2-氯乙基)酯残余化学物)的全二维气相色谱-飞行时间质谱(GC×GC-TOF MS)检测方法。样品裁剪后经甲醇超声萃取,萃取液氮吹浓缩至2 mL,用GC×GC-TOF MS检测,飞行时间质谱定性,外标法定量。结果显示,50种高关注物质在0.05~15 mg/L质量浓度范围内线性关系良好,相关系数(r2)不低于0.990 4,方法的检出限(LOD)和定量下限(LOQ)分别为0.04~5.96 mg/kg和0.05~13.39 mg/kg,在低、中、高3个加标浓度下的回收率为80.0%~121%,相对标准偏差(RSD,n=6)为1.1%~13%。将该方法用于实际样品检测,检出邻苯二甲酸酯和多环芳烃。方法准确、高效,可同时实现50种高关注物质的筛查和确证。
中文关键词:全二维气相色谱-飞行时间质谱(GC×GC-TOF MS)  塑料  高关注物质(SVHC)
 
Determination of 50 Substances of Very High Concern in Plastic by Comprehensive Two-dimensional Gas Chromatography-Time-of-flight Mass Spectrometry
Abstract:A two-dimensional gas chromatography-time of flight mass spectrometry(GC×GC-TOF MS) was developed for the determination of 50 substances of very high concern(SVHCs) in plastic,including 24 polycyclic aromatic hydrocarbons,17 phthalates,3 alkyl phenols,4 benzotriazole ultraviolet stabilizers,karanal and triphosphate(2-chloroethyl) ester.Samples were shattered and extracted with methanol by ultrasonic extraction.The qualitative analyses were performed by TOF MS.The quantitative analyses were performed by external standard method.Results showed that there were good linear relationships for 50 analytes in the concentration range of 0.05-15 mg/L with their correlation coefficients(r2) not less than 0.990 4.The limits of detection(LODs) and limits of quantitation(LOQs) were in the ranges of 0.04-5.96 mg/kg and 0.05-13.39 mg/kg,respectively.The recoveries at low,medium and high spiked levels ranged from 80.0% to 121% with relative standard deviations(RSDs,n=6) of 1.1%-13%.Phthalates and Polycyclic aromatic hydrocarbons were detected when this method was applied to the detection for real samples.This method could be used for the simultaneous screening and confirmation of 50 SVHCs in plastic with accuracy and efficiency.
Key Words:two-dimensional gas chromatography with time of flight mass spectrometry(GC×GC-TOF MS)  plastic  substance of very high concern(SVHC)
引用本文:周龙龙,薛秋红,刘一龙,牛增元,罗忻,尹桂林,马强,谢堂堂.全二维气相色谱-飞行时间质谱法测定塑料中50种高关注物质[J].分析测试学报,2020,39(12):1458-1465.
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