有机试剂4-(6-甲氧基-8-喹啉偶氮)-间苯二酚的合成和结构分析

以 6-甲氧基 - 8-氨基喹啉为原料 ,经重氮化后与间苯二酚偶联 ,合成了有机试剂 4- (6-甲氧基 - 8-喹啉偶氮 ) -间苯二酚 (简称 MQAR) ,用 DMF重结晶精制。通过TL C、EA、UV- VIS、IR、1 HNMR等分析手段 ,对合成产物进行分析和结构鉴定 ,确证得到了 MQAR纯品 ,产品熔点为 1 94℃。     

Coprecipitation with Cu(II)‐4‐(2‐Pyridylazo)‐resorcinol for Separation and Preconcentration of Fe(III) and Ni(II) in Water and Food Samples

The coprecipitation method is widely used for the preconcentration of trace metal ions prior to their determination by flame atomic absorption spectrometry (FAAS). A simple and sensitive method based on coprecipitation of Fe(III) and Ni(II) ions with Cu(II)‐4‐(2‐pyridylazo)‐resorcinol was developed. The analytical parameters including pH, amount of copper (II), amount of reagent, sample volume, etc., were examined. It was found that the metal ions studied were quantitatively coprecipitated in the pH range of 5.0–6.5. The detection limits (DL) (n = 10, 3s/b) were found to be 0.68 µg L^?1 for Fe(III) and 0.43 µg L^?1 for Ni(II) and the relative standard deviations (RSD) were ≤4.0%. The proposed method was validated by the analysis of three certified reference materials (TMDA 54.4 fortified lake water, SRM 1568a rice flour, and GBW07605 tea) and recovery tests. The method was successfully applied to sea water, lake water, and various food samples.     

Humic substances,a possible source of environmental goitrogens

The by-products of humic substances (HS), resorcinol, orcinol, phloroglucinol, pyrogallol, 3,4- and 3,5-dihydroxybenzoic acids, and ortho- and meta-phthalic acids, have been tested for antithyroid and goitrogenic activities. By two in vitro assays all compounds, except the phthalic acids, were potent inhibitors of the thyroid peroxidase enzyme, and of thyroidal ¹²⁵I uptake and/or its incorporation into thyroid hormones using thyroid slices. Resorcinol in drinking water was goitrogenic as indicated by in vivo assay in rats. These findings, the identification of resorcinol in the water supply of an endemic goiter district in western Colombia, where increased goiter prevalence is associated with watersheds rich in organic matter, and results of elemental analysis of goitrogenic water extracts from the same district showing a composition similar to that of aquatic HS, suggest that HS degradation by-products may play an important role in the etiology of endemic goiter.