加速溶剂萃取-高效液相色谱-电感耦合等离子体质谱法测定聚乳酸材料中4种有机锡化合物

建立了加速溶剂萃取-高效液相色谱-电感耦合等离子体质谱（ASE-HPLC-ICP-MS）测定聚乳酸材料中二丁基锡（DBT）、三丁基锡（TBT）、三苯基锡（TPhT）、二辛基锡（DOT）4种有机锡化合物的方法。采用加速溶剂萃取法，以V(甲醇)∶V（水）∶V（乙酸）=65∶23∶12的溶液为提取溶剂，于120 ℃静态萃取10 min，萃取液定容后，以Agilent TC-C18液相色谱柱为分离柱，甲醇-35%乙酸水溶液（3.0%三乙胺）作为流动相进行梯度洗脱，ICP-MS测定。结果表明：DBT、TPhT、TBT在质量浓度为1~100 μg/L、DOT在质量浓度为3~300 μg/L范围内，具有良好的线性关系（r²≥0.999）；DBT、TPhT、TBT、DOT的定量限分别为30.0、33.3、55.0、101.7 μg/kg；在定量限、5倍定量限和参照Oeko-tex Standard 100限量值3个加标水平下，平均回收率分别为82.7%~88.4%、89.5%~91.5%、91.6%~103.5%，相对标准偏差（RSDs）为4.3%~7.8%。该方法简单、灵敏、准确，各项技术指标均满足国内外相关法规的要求，可用于聚乳酸材料中有机锡化合物残留的确证检测。

Determination of Four Organotin Compounds in Poly(Lactic Acid) Materials by ASE-HPLC-ICP-MS

A method was developed for the determination of four organotin compounds including dibutyltin(DBT), triphenyltin(TPhT), tributyltin(TBT) and dioctyltin(DOT) in poly(lactic acid) materials by accelerated solvent extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometer(ASE-HPLC-ICP-MS). The crushed samples were extracted for 10 min under 120 ℃ by ASE， methanol-water-acetic acid mixture（65∶23∶12，V/V/V） as the extraction solvent. The filtered extract was eluted on Agilent TC-C18 column using the mobile phase of methanol and 35% acetic acid aqueous solution(3.0% triethylamine) gradient elution, which was determined by ICP-MS. The mass concentration of organotin compounds has a linear range of 1-100 μg/L for DBT, TPhT and TBT, 3-300 μg/L for DOT with good correlation coefficients (r²≥0.999). The limits of quantitation (LOQs) are 30.0, 33.3, 55.0, 101.7 μg/kg for DBT, TPhT, TBT and DOT, respectively. The average spiked recoveries are 82.7%-88.4%， 89.5%-91.5%， 91.6%-103.5% at the level of LOQ, five times the LOQ and the limit values of Oeko-tex Standard 100， respectively, with the relative standard deviations(RSDs) of 4.3%-7.8%. The method is simple, effective, reliable and highly sensitive, which can meet the requirements of the domestic and international legislations，and can be used to determine organotin residues in poly(lactic acid) materials.