US EPA

1173027 

Journal Article 

Determination of organotin compounds in biological samples using ethyl derivatization and GC/MS 

Iwamura, T; Kadokami, K; Jin-Ya, D; Tanada, K 

2000 

1 

Bunseki Kagaku / Analysis Chemistry
ISSN: 0525-1931 

Japan Society for Analytical Chemistry 

TOKYO 

49 

7 

523-528 

Japanese 

10.2116/bunsekikagaku.49.523 

WOS:000088462800006 

A method for the simultaneous determination of organotins (monobutyl- ,dibutyl-, tributyl-, monophenyl-, diphenyl- and triphenyltin) in biological samples has been developed using ethyl derivatizaion and isotope dilution GC/MS. After the addition of deuterated organotins as internal standards to a homogenized biological sample, organotin compounds were extracted with 1 M HBr-methanol/ethyl acetate (1 : 1); the extract was filtered and added to a saturated NaBr solution. The sample solution was then extracted with ethyl acetate/hexane (3 : 2), and the extract was mixed with hexane. The organic layer was dehydrated and concentrated. The concentrate was mixed with a buffer solution (pH 5.0) and NaBEt4 solution to derivatize target organotins. Then, 1 M KOH-ethanol was added to the derivatized sample solution and the mixture was shaken for 1 hour to decompose any fat. After saponification, ethylated organotins were extracted with hexane, and the extract was first dehydrated and then concentrated. The sample was cleaned up using a florisil cartridge column. Determination was carried out by GC/MS-SIM. The results of overall recovery tests at μg/kg levels showed that the mean recovery was 123% and their mean relative standard deviation was 12.5%. The detection limits of the method ranged from 0.13 to 6.6 μg/kg. 

organotin; biological sample; ethylation; isotope dilution GC/MS