固相萃取-气相色谱／质谱法同时测定涂料中的8种有机锡

Simultaneous Determination of Eight Organotin Compounds in Coatings by Solid Phase Extraction (SPE) and Gas Chromatography/Mass Spectrometry

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5mL甲醇、7mL洗脱液（氯化铵、甲醇、冰乙酸的混合溶液）预洗，10mL甲醇活化；将用甲醇稀释的涂料样品上样后，用5mL甲醇淋洗，抽干2min，7mL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％。

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）.