Kawakami Tsuyoshi, Isama Kazuo, Nakashima Harunobu, Ooshima Tomoko, Tsuchiya Toshie, Matsuoka Atsuko
Division of Medical Devices, National Institute of Health Sciences, Tokyo, Japan.
Yakugaku Zasshi. 2010 Feb;130(2):223-35. doi: 10.1248/yakushi.130.223.
The use of tributyltin (TBT) and triphenyltin (TPT) in some household products are prohibited by "Act on the Control of Household Products Containing Harmful Substances" in Japan. In this study, methods for determination of TBT and TPT in water soluble paints and adhesives were developed by GC-MS. These compounds in paints and adhesives, which were mainly composed of vinyl acetate, urethane and acryl resins, and chloroprene rubber, were firstly extracted with HCl-acetone, and then extracted with hexane. On the other hand, the adhesive composed of natural rubber was firstly dispersed in water before acidification. The organotins were extracted with hexane from this solution and then these compounds were extracted with acetonitrile from hexane extract. These extracts were purified by a florisil cartridge column after ethyl-derivation with sodium tetraethylborate, and analyzed by GC-MS. The quantifications using deuterated compound of both organotins as surrogate standard were conducted, and good results were obtained. The recoveries were 81 to 118% and the coefficients of variation were 0.83 to 4.3% (TBT and TPT added; 5 microg/g). The method quantification limits were 0.0090 to 0.025 microg/g, which were lower than those of an official method. These methods were applied to monobutyltin (MBT), dibutyltin (DBT), monophenyltin (MPT), and diphenyltin (DPT). DBT and DPT in paints and adhesives were quantified, except for DPT in natural rubber. These methods were applied to commercial products. DBT was detected at low concentrations (t.r.-0.19 microg/g) in some paint samples, while TBT and TPT were not detected in all samples.
在日本,《含有有害物质的家用产品控制法》禁止在某些家用产品中使用三丁基锡(TBT)和三苯基锡(TPT)。在本研究中,采用气相色谱 - 质谱联用(GC-MS)技术开发了测定水溶性涂料和胶粘剂中TBT和TPT的方法。涂料和胶粘剂中的这些化合物主要由醋酸乙烯酯、聚氨酯和丙烯酸树脂以及氯丁橡胶组成,首先用盐酸 - 丙酮进行萃取,然后用己烷萃取。另一方面,由天然橡胶组成的胶粘剂在酸化前先分散于水中。从该溶液中用己烷萃取有机锡,然后从己烷萃取物中用乙腈萃取这些化合物。在用四乙基硼酸钠进行乙基衍生化后,这些萃取物通过弗罗里硅土柱进行净化,并通过GC-MS进行分析。使用两种有机锡的氘代化合物作为替代标准进行定量,获得了良好的结果。回收率为81%至118%,变异系数为0.83%至4.3%(添加TBT和TPT;5μg/g)。方法定量限为0.0090至0.025μg/g,低于官方方法的定量限。这些方法也适用于一丁基锡(MBT)、二丁基锡(DBT)、一苯基锡(MPT)和二苯基锡(DPT)。对涂料和胶粘剂中的DBT和DPT进行了定量,天然橡胶中的DPT除外。这些方法应用于商业产品。在一些涂料样品中检测到低浓度(保留时间 - 0.19μg/g)的DBT,而在所有样品中均未检测到TBT和TPT。