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用四乙基硼酸钠进行乙基衍生化后,采用气相色谱/质谱法测定塑料制品中的有机锡化合物

[Determination of organotin compounds in plastic products by GC/MS after ethyl derivatization with sodium tetraethylborate].

作者信息

Ohno Hiroyuki, Suzuki Masako, Nakashima Shigehito, Aoyama Taiki, Mitani Kazunori

机构信息

Nagoya City Public Health Research Institute: 1-11, Hagiyama-cho, Mizuho-ku, Nagoya 467-8615, Japan.

出版信息

Shokuhin Eiseigaku Zasshi. 2002 Aug;43(4):208-14. doi: 10.3358/shokueishi.43.208.

Abstract

A simultaneous determination method for 9 organotin compounds in polyvinyl chloride (PVC) and silicone products used as kitchen utensils and food packages was developed using ethyl derivatization with sodium tetraethylborate (NaBEt4). Organotin compounds were extracted with acetone-hexane (3:7) from the samples after acidification and the extract was filtered and concentrated at under 40 degrees C. After centrifugal separation, these compounds were derivatized with 2% NaBEt4 solution and determined by GC/MS. This method was applicable for simple routine analysis. Recoveries of spiked compounds were 49.1-118.1% for 3 PVC products and 88.8-102.2% for a siliconized paper. Monooctyltin, dioctyltin and trioctyltin compounds were found in all PVC food containers at the levels of 123-1,380 micrograms/g, 1,770-13,200 micrograms/g and 6.6-139 micrograms/g, respectively. They also were found in 3 gloves, 5 spouts, 1 hose and 5 pipes. Some PVC products contained monomethyltin, dimethyltin, trimethyltin, monobutyltin and dibutyltin compounds at the levels of 97.3-433 micrograms/g, 96.5-5,120 micrograms/g, 8.5-24.9 micrograms/g, 1.2-852 micrograms/g and 1.2-29.4 micrograms/g, respectively.

摘要

建立了一种同时测定用作厨房用具和食品包装的聚氯乙烯(PVC)及硅酮产品中9种有机锡化合物的方法,该方法采用四乙基硼酸钠(NaBEt4)进行乙基衍生化。样品经酸化后,用丙酮 - 己烷(3:7)萃取有机锡化合物,萃取液过滤后在40℃以下浓缩。离心分离后,这些化合物用2%的NaBEt4溶液进行衍生化,并用气相色谱/质谱联用仪(GC/MS)测定。该方法适用于简单的常规分析。3种PVC产品中加标化合物的回收率为49.1% - 118.1%,硅油纸的回收率为88.8% - 102.2%。在所有PVC食品容器中均检测到单辛基锡、二辛基锡和三辛基锡化合物,含量分别为123 - 1380微克/克、1770 - 13200微克/克和6.6 - 139微克/克。在3只手套、5个喷口、1根软管和5根管道中也检测到了它们。一些PVC产品中还含有一甲基锡、二甲基锡、三甲基锡、一丁基锡和二丁基锡化合物,含量分别为97.3 - 433微克/克、96.5 - 5120微克/克、8.5 - 24.9微克/克、1.2 - 852微克/克和1.2 - 29.4微克/克。

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