贝类水产品中有机锡和甲基汞的检测研究

Detection and analysis of organotin and methyl-mercury in aquatic products of shellfish

目的建立贝类水产品中甲基汞、三甲基锡(TMT)、一丁基锡(MBT)、二丁基锡(DBT)、三丁基锡(TBT)和三苯基锡(TPhT)等6种有机锡和甲基汞化合物的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)的分离检测方法。方法利用Eclipse Plus C18反相色谱柱对贝类水产品中6种有机金属化合物进行分离,利用电感耦合等离子体质谱对锡和汞元素进行检测,外标法定量测定水产品中6种有机金属化合物的含量。通过优化色谱分离条件,以甲醇-0.06 mol/L乙酸铵-乙酸溶液为流动相,梯度洗脱。结果 6种有机金属化合物在30 min内得到了有效分离。6种有机金属化合物标准曲线的线性相关系数大于0.998,检出限为0.5~2.5μg/kg,样品加标回收率在70%~110%。结论该法操作简便,分离效果好,检出限低,适用于贝类水产品中有机锡和甲基汞的检测。

Objective To establish a method for determination of methyl-mercury and five organotin (TMT, MBT, DBT, TBT, TPhT) in aquatic products of shellfish using high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS). Methods An Eclipse Plus C18 column with methanol-0.06 mol/L ammonium acetate-acetate acid as mobile phased was used to separate the six compounds, and the content of these six compounds was carried out by external standard method using plasma mass spectrometry. Results The 6 compounds were effectively separated in 30 mins. The linear correlation coefficient of the standard curve of 6 kinds of organic metal compound was larger than 0.998, the detection limit was 0.5~2.5 μg/kg, and the spiked recoveries ranged from 70% to 110%. Conclusion The method is a simultaneous determination for organotin and methyl-mercury in aquatic products of shellfish with simple and convenient operation, efficient separation and low detection limit.