Shingo Hirao, H. Hasegawa, K. Mori, Hidetomo Yamamori
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引用次数: 0
摘要
建立了液相色谱串联质谱法(LC-MS / MS)分析沉积物中聚氨基甲酸酯的方法。在这种方法中，沉淀物中的聚氨基甲酸酯被甲基化成乙二硫代氨基甲酸二甲基(EBDC- 2 Me)和二甲基二硫代氨基甲酸二甲基(DMDC-Me)。聚氨基甲酸酯的浓度由EBDC- 2me计算得到。方法检出限(MDL)和定量限(MQL)均为0。94纳克/克干和2。57 ng / g-dry。沉积物平均回收率为77。8%，相对标准偏差(RSD)为2。1%。在富有机物沉积物中加入甲醇作为溶剂萃取，提高了萃取回收率。将聚氨基甲酸酯添加到沉积物中，在保存一天后完全消失。相比之下，添加到粗提物中的聚氨基甲酸酯在保存3天内几乎是稳定的，而在保存7天时则完全丢失。在名古屋市采样的河流和海洋沉积物中聚氨基甲酸酯的浓度低于MDL。
A Study on the Development of Analytical Method for Polycarbamate by LC-MS/MS and its Decomposition Property in Sediment
An analytical method for polycarbamate in sediment by liquid chromatography tandem-mass spectrometry (LC-MS / MS) was developed. In this method, polycarbamate in sediment is methylated to ethylenebis dithiocarbamate dimethyl (EBDC- 2 Me) and dimethyldithiocarbamate methyl (DMDC-Me). Concentrations of polycarbamate are calculated from that of EBDC- 2 Me. The method detection limit (MDL) and method quantification limit (MQL) were 0 . 94 ng / g-dry and 2 . 57 ng / g-dry, respectively. The average recovery rate from sediment were 77 . 8 % with a relative standard deviation (RSD) of 2 . 1 %. Recovery rate was improved by the addition of methanol as solvent extraction in the case of organic-rich sediments. Polycarbamate added to sediment was completely lost for a day of preservation. In contrast, polycarbamate added to the crude extract was almost stable for three days of preservation, while it was completely lost for seven days of preservation. The concentrations of polycarbamate in the river and sea sediments sampled at Nagoya city were below the MDL.
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