The gas chromatography of the heptafluorobutyryl derivatives of carbofuran, 3-ketocarbofuran and 3-hydroxycarbofuran is examined with electrolytic conductivity detection (halogen mode). The reaction consists of heating the compounds with heptafluorobutyric anhydride in the presence of trimethylamine
Detection of goitrin and its heptafluorobutyryl derivative by gas—liquid chromatography with electron capture, electrolytic conductivity and sulfur detectors
✍ Scribed by H.A. McLeod; G. Benns; D. Lewis; J.F. Lawrence
- Publisher
- Elsevier Science
- Year
- 1978
- Tongue
- English
- Weight
- 392 KB
- Volume
- 157
- Category
- Article
- ISSN
- 1873-3778
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✦ Synopsis
The separation of goitrin by two gas-liquid cbromatographic columns, the response of different detectors and the use of the heptafluorobutyric (HFB) anhydride derivative of goitrin to improve sensitivity was investigated. The non-polar 3 % OV-1 and the intermediate 4% SE-30/6% SP-2401 on SO-100 mesh Chromosorb W HP g&e comparable results and were considered interchangeable. The sensitivities of the electron capture, sulfur 394 nm emission, chlorine and nitrogen Coulson electrolytic conductivity detectors were inadequate for goitrin per se. Chromatography and sensitivity of all detectors to goitrin were greatly improved by using by using the HFB derivative. It was possible to detect 1 to 60 ng of goitrin-HFB in standard solutions. Application of the technique to go&n-spiked (2 ppm) milk, cleaned up by high-performance liquid chromatography, encountered no problems and was considered satisfactory for all four detectors. l-NTRODUCTKON Go&in, I,%vinyloxazolidine-2-thione (Fig. l), is the aglycone hydrolysis product of progoitrin, a glucosinolate found in rape, turnip and cabbate'>. Go&in is similar to thiouracil in antithyroid activity I. The presence of this compound in foods for human consumption is of some concern to health authorities since residues may occur in milk and other products from animals fed with rapeseed meal protein supplements5-7.
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