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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 6 kinds of organotin such as methylmercury, trimethyltin (TMT), monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT) and triphenyltin (TPhT) High performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) separation and detection of methylmercury compounds. Methods Six kinds of organometallic compounds in shellfish aquatic products were separated by Eclipse Plus C18 reversed-phase column. The content of tin and mercury in the shellfish aquatic products were determined by inductively-coupled plasma mass spectrometry. The contents of six organometallic compounds Content. By optimizing the conditions of chromatographic separation, a gradient of methanol-0.06 mol / L ammonium acetate-acetic acid was used as the mobile phase. Results Six kinds of organometallic compounds were effectively separated within 30 min. The calibration curves of six organometallic compounds showed a linear correlation coefficient of greater than 0.998 with a detection limit of 0.5-2.5 μg / kg and spiked recoveries of 70% -110%. Conclusion The method is simple and convenient to operate and has good separation effect and low detection limit. It is suitable for the detection of organotin and methyl mercury in shellfish aquatic products.