【摘要】 建立了一种固相萃取(SPE)前处理、气相色谱-质谱(GC-MS)法同时测定涂料中8种有机锡的方法。样品采用阳离子交换固相萃取小柱净化,最佳固相萃取条件为:固相萃取小柱分别用5 mL甲醇、7 mL洗脱液(氯化铵、甲醇、冰乙酸的混合溶液)预洗,10 mL甲醇活化;将用甲醇稀释的涂料样品上样后,用5 mL甲醇淋洗,抽干2 min,7 mL乙酸-氯化铵甲醇溶液(10∶90,V/V)洗脱溶液洗脱。洗脱液用四乙基硼化钠溶液衍生后,气相色谱-质谱法进行定性定量分析。结果表明:以标准加入法计算回收率,在1.68%~16.84%添加范围内,平均回收率在85%~105%之间,相对标准偏差均小于12%。更多还原

【Abstract】 The method of simultaneous determination of eight organotin compounds in coatings with solid phase extraction(SPE)-gas chromatography/mass spectrometry(GC/MS) was described.Before cleaned up with a SCX cartridge,the coating samples were diluted successively with ethyl acetate and methanol.The purification conditions were optimized.The SCX SPE cartridge was conditioned successively by 5 mL methanol,7 mL acetic acid-ammonium chloride solution and 10 mL methanol.After rinsed with 5mL methanol,sample was eluted with 7 mL acetic acid-ammonium chloride solution with the ratio of 10∶90(V/V).The resulting elutes were deraivatized with NaBEt4,and analysed with gas chromatography/mass spectrometry.Precise and recoveries of entire procedure were evaluated by standard addition method.The average recoveries ranged from 85% to 105% with the relative standard deviations below 12% at a spiking level from 1.68% to 16.84%(n=7).更多还原