Simultaneous determination of methyl mercury, ethyl mercury and tributyltin in seawater by gas chromatography-mass spectrometry
HUANG Jian, ZHANG Wenguo, SHI Jinhui, CAO Haifeng, WANG Hongwei, GE Hongmei, WANG Jinjuan
Nantong Customs Comprehensive Technology Center, Nantong 226004, China
摘要：建立气相色谱-质谱法同时测定海水中甲基汞、乙基汞和三丁基锡的分析方法。海水样品用乙酸调节pH后，用四苯基硼酸钠进行衍生，经HP-5MS毛细柱分离，选择离子监控(SIM)模式检测，以外标法定量。甲基汞、乙基汞和三丁基锡的质量浓度在0.1～2 mg/L范围内与色谱峰面积呈良好的线性关系，相关系数均大于0.998，检出限分别为0.015，0.015，0.010 mg/L，样品平均加标回收率为78.1%～90.2%，相对标准偏差为2.3%～4.5%(n=6)。该方法前处理简单，可用于海水中有机汞和有机锡的同时测定。
Abstract：A method for the simultaneous determination of methyl mercury, ethyl mercury and tributyltin in seawater by gas chromatography-mass spectrometry(GC-MS) was established. The pH of seawater samples was adjusted by acetic acid. The samples were derived by sodium tetrapenylborate and then separated by HP-5MS(30 m×0.25 mm, 0.25 μm)column, finally determined by GC-MS with selected ion monitoring and quantified with external standard method. The mass concentrations of methyl mercury, ethyl mercury and tributyltin had a good linear relationship with the chromatographic peak area in the range of 0.1-2 mg/L, the correlation coefficients were all more than 0.998, and the detection limits were 0.015, 0.015 and 0.010 mg/L, respectively. The average recoveries were 78.1%-90.2%, and the relative standard deviations were 2.3%-4.5%(n=6). The method is simple in pretreatment, which can be used for simultaneous determination of organomercury and organotin in seawater.
Keywords：gas chromatography-mass spectrometry; organomercury; organotin
HUANG J，ZHANG W G，SHI J H，et al. Simultaneous determination of methyl mercury，ethyl mercury and tributyltin in seawater by gas chromatography-mass spectrometry[J]. Chemical analysis and meterage，2020，29(6)：51-54.