A specific chromatographic LC/MS/MS assay is described for the confirmatory identification of residues of sarafloxacin, an arylfluoroquinolone antibacterial agent, in catfish tissue. This confirmatory method takes advantage of the specificity provided by sample preparation, liquid chromatography, and tandem mass spectrometry. This kind of multidimensional analysis is commonly used in environmental, pharmacokinetic, residue, and other studies. However, we demonstrate the addition of a previously unreported criterion, the use of ion ratio ranges from the tandem mass spectrometry (MS/MS) experiment as an aid in confirmation. Using the described method, we were able to achieve MS/MS product ion ratios with <7% variation during 1 day of analysis for over 25 injections. We believe the addition of this criterion will increase the scientific certainty of the confirmatory method.
5-Bromotryptophan (5-BrTrp) is the most potent amino acid derivative reported in the literature to inhibit the gelation of hemoglobin S (from sickle cell anemia patients). Trp-Trp is also more potent than Trp as an antigelation agent. Therefore, we have prepared a series of dipeptides containing 5-BrTrp and evaluated the antigelation activity. 5-BrTrp-5-BrTrp is the most potent, i.e., 5.9 times the activity of Trp, followed by 5-BrTrp-Trp and then Trp-5-BrTrp. This improved antigelation potency for 5-BrTrp-5-BrTrp and 5-BrTrp-Trp is very significant and will be pursued further as lead compounds with potential for sickle cell anemia.
A series of N‐1 or C‐2 phenylalkyl substituted tryptophans and C‐1 phenylalkyl substituted 3,4‐dihydro‐β‐carbolines were prepared from the apropriate aniline, 1b or 1e, or tryptophan, 8 or 11, by ring closure methods. None of the compounds prepared were more potent than 5‐bromotryptophan (11) as inhibitors of sickle cell hemoglobin gelation.
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