Simultaneous Determination of Multi-Organotin Compounds in Seawater by Liquid-Liquid Extraction-High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry
1. Institute of Oceanology，Chinese Academy of Sciences, Qingdao 266071, China 2. Graduate University of Chinese Academy of Sciences, Beijing 100049, China 3. Qingdao Center for Disease and Prevention, Qingdao 266033，China 4. First Institute Oceanography of State Oceanic Adiministration, Qingdao 266061, China 5. Agilent Company in China, Beijing 100022, China
Abstract：The hyphenated technique of high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) was applied to the simultaneous determination of five organotin compounds (trimethyltin, dibutyltin, tributyltin, diphenyltin and triphenyltin) in seawater samples. Agilent TC-C18 column was used for the separation, the mobile phase of HPLC was CH3CN∶H2O∶CH3COOH=65∶23∶12 (φ)，0.05% TEA, and pH value was adjusted to 3.0 by diluent ammonia. The flow rate was 0.6 mL·min-1. Five mixed organotin compounds in a mix standard solution from 100 to 0.5 μg·L-1 were applied for the method assessment. The experimental results indicate that the correlation coefficient of calibration curves (R2) for each organotin compound was over 0.998 and the detection limits of the five organotin compounds were lower than 3 ng·L-1. Different mixed organic solvents including dichloromethane or toluene were used for extraction of organotin and the extraction condition of organotin from seawater was optimized. The 100 mL seawater acidized by hydrochloric acid was extracted by 10 mL carbon dichloride (CH2Cl2) with 2% tropolone for 10 min twice. Extracted organic solvents were mixed and blown to one drop by nitrogen with the rate of 1.7 mL·min-1, then 1 mL acetonitrile was added to the drop for redissolving the organotin compounds. Finally, the mixed redissolution was filtered by 0.22 μm organic filter membrane before analysis. It was found that the only organotin compound in seawater was triphenyltin (TPHT) and the content was 53.2 ng·L-1. The recoveries test from the standard addition for diphenyltin (DPHT), dibutyltin (DBT), tributyltin (TBT) and triphenyltin (TPHT) were over 80%. However, the recovery for trimethyltin (TMT) was relatively low and the value was 50%. The reason might be attributed to the decomposition or adsorption of those compounds during the extraction procedure. Further study on this subject is in progress.
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