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M1,as a main metabolite appeared in bile and urine,was calculated as C19H23FN4O4 by the Formula Predictor software according to the accurate mass.Thus,M1 (addition of CH2 to M0)was preliminary concluded as the methylating product of M0.In order to pinpoint the site of methylation in this metabolite,we compared the 多级质谱[打不出来符号，只能打汉字了]data from M1 with the corresponding data of the parent drug.The fragment obtained from the precursor(m/z 391.1774) showed a major product ion at m/z 359.1503,which could lead to six MS3[三级质谱] product ions at m/z 331.1557,302.0837,283.0941,214.0880,201.1025 and 184.0888.On the basis of the elemental compositions of fragment ions and bond connectivities present in the parent molecule,the most likely methylating position was located at the carboxyl group.The possible structure and proposed fragmentation pathways of M1 are shown in Fig.4. The molecular ion of M2(m/z 407.1724,C19H23FN4O5) was 15.9950 Da higher than that of the molecular ion of M1 and its main product ions at m/z 348.1236 and 293.0906.Calcilating the formula by the Formula Predictor software ,the product ions at m/z 348.1236 and 293.0906 were formed through neutral losing of C2H5NO and C5H10N2O,respectively.In fact,the key fragment ion(m/z 293.0906) had permitted rapid localization of the site of hydroxylation on the N-methylpiperazine.The possible struture and proposed fragmentation pathways of M2 can be seen clearly from Fig.4. |
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2楼2016-01-28 17:01:52
