高效液相色谱-电感耦合等离子质谱法分析水产品中有机锡的形态

Speciation Analysis of Organotins in Aquatic Products by High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry

建立了水产品中三甲基锡（TMT）、一丁基锡（MBT）、二丁基锡（DBT）、三丁基锡（TBT）、一苯基锡（MPh T）、二苯基锡（DPh T）、三苯基锡（TPh T）7种有机锡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反相色谱柱对水产品中7种有机锡化合物进行分离,利用电感耦合等离子体质谱对锡元素进行检测,外标法定量测定水产品中7种有机锡化合物的含量。研究采用30 m L 30%乙酸-甲醇提取液（V/V）,低温超声萃取10 min后离心3 min,取上清液20 m L浓缩,用流动相定容至2 m L,以乙酸（0.2%三乙胺,V/V）-甲醇溶液为流动相,梯度洗脱,7种有机锡化合物在30 min内得到了有效分离。7种有机锡化合物标准曲线的线性相关系数大于0.995,检出限0.11-0.60μg/kg。此前处理方法样品加标回收率为72.1%-111.7%。本方法操作简便,分离效果好,检出限低,适用于水产品中有机锡的检测。

A method for determination of seven organotins（ TMT,MBT,DBT,TBT,MPh T,DPh T,TPh T）in aquatic products was established using high performance liquid chromatography-inductively coupled plasmamass spectrometry（ HPLC-ICP-MS）. An Eclipse Plus C18 column was used to separate the seven compounds using methanol-acetic acid（ with 0. 2% triethylamine V / V） acid as the mobile phase,and the contents of these seven compounds were determined by external standard method using plasma mass spectrometry. The seven organotins compounds were effectively extracted using 30 m L of 30%（ V / V） acetic acid-methanol with ultrasound for 10 min in low temperature,centrifuged for 3 min and the 20 m L supernatant was concentrated and diluted with mobile phase to 2 m L,and then separated in 30 min with gradient elution. Linear correlation coefficient for the standard curve of seven kinds of organotins was larger than 0. 995,and detection limit was0. 11- 0. 60 μg / kg. The spiked recoveries ranged from 72. 1% to 111. 7%. The method is feasible for the simultaneous determination of organotins in aquatic products with simple and convenient operation,efficient separation and low detection limit.