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前吸附技术-超高压液相色谱-串联质谱法同时测定酒中24种邻苯二甲酸酯
引用本文:吴敏,郑向华,张志刚,陈燕,林立毅,黄志强. 前吸附技术-超高压液相色谱-串联质谱法同时测定酒中24种邻苯二甲酸酯[J]. 色谱, 2016, 34(7): 673-680. DOI: 10.3724/SP.J.1123.2016.03001
作者姓名:吴敏  郑向华  张志刚  陈燕  林立毅  黄志强
作者单位:1. 厦门出入境检验检疫局, 福建 厦门 361026;2. 湖南省检验检疫科学技术研究院, 湖南 长沙 410004
基金项目:"十二五"国家科技支撑计划项目(2012BAK08B01);福建省自然科学基金项目(2014J01057).
摘    要:建立了前吸附技术-超高压液相色谱-串联质谱测定酒中24种邻苯二甲酸酯含量的方法。酒类样品经稀释、净化后采用前吸附技术排除仪器管路中的本底干扰,经超高压液相色谱-串联质谱仪进行测定。采用多反应监测模式、电喷雾电离源正离子(ESI+)模式进行检测,外标法定量。24种邻苯二甲酸酯在0.005~2.00 mg/L范围内线性关系良好,相关系数(r)均大于0.99,检出限(S/N=3)为0.003~0.05 mg/kg。以不含增塑剂的酒类样品作为空白样品进行加标回收率试验,各种邻苯二甲酸酯化合物的回收率为75.4%~118.2%,相对标准偏差(RSD)为4.0%~11.2%。该法不但可以有效排除管路中邻苯二甲酸酯本底的干扰,而且简单、灵敏、稳定。

关 键 词:超高压液相色谱-串联质谱    邻苯二甲酸酯  前吸附技术  
收稿时间:2016-03-03

Simultaneous determination of 24 phthalates in liquors using front adsorption technology and ultra performance liquid chromatography-tandem mass spectrometry
WU Min,ZHENG Xianghua,ZHANG Zhigang,CHEN Yan,LIN Liyi,HUANG Zhiqiang. Simultaneous determination of 24 phthalates in liquors using front adsorption technology and ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese journal of chromatography, 2016, 34(7): 673-680. DOI: 10.3724/SP.J.1123.2016.03001
Authors:WU Min  ZHENG Xianghua  ZHANG Zhigang  CHEN Yan  LIN Liyi  HUANG Zhiqiang
Affiliation:1. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China;2. Hunan Inspection and Quarantine Technology Academy, Changsha 410004, China
Abstract:A method for the simultaneous determination of 24 phthalates in liquors was developed by using front adsorption technology and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were diluted and cleaned-up by an HLB solid phase extraction cartridge. The front adsorption technology was used to suppress the interferences which came from plastic pipes in the UPLC-MS/MS. And then the targets were analyzed by UPLC-MS/MS under the positive ion mode using multiple reaction monitoring (MRM) mode. The calibration curves showed a good linearity in the range of 0.005-2.00 mg/L with r>0.99. The limits of detections (S/N=3) were 0.003-0.05 mg/kg. The average recoveries of the spiked samples were between 75.4% and 118.2% with the relative standard deviations (RSDs) of 4.0%-11.2%. The method could be used to simultaneously confirm the multi-residue of the 24 phthalates in liquors. And the method is simple, sensitive and stable.
Keywords:front adsorbing technology  liquors  phthalates  ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)  
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