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Positive- and negative-ion mass spectrometry of diphenylmethane antihistaminics and their analogues and rapid clean-up of them from biological samples.
Forensic Sci Int. 1993 Dec; 62(3):187-208.FS

Abstract

Positive-ion electron impact (PIEI), positive-ion chemical ionization (PICI) and negative-ion chemical ionization (NICI) mass spectra are presented for 15 compounds of diphenylmethane antihistaminics and their analogues, and each fragmentation pathway was analyzed. In the PIEI mode, molecular peaks were very small or missing for most compounds. Peaks at m/z 58, due to a dimethylaminomethyl group liberated, constituted base peaks in five compounds. Peaks at m/z 165 and/or 167, due to diaromatic rings plus a methyl group, appeared in most compounds. In the PICI mode, peaks due to M+H and M+C2H5 appeared in all compounds. Peaks due to diaromatic rings plus a methyl or ethyl group constituted base peaks in five compounds, which had an ether bond in their structures. In the NICI mode, anions at m/z M-H appeared in most compounds. Peaks at m/z 35 were observed for compounds having a chlorine group in their structures. Detection limits for total ion monitoring of these compounds were 20-50 ng on column in the PIEI mode, 100-200 ng in the PICI mode and 500-1000 ng in the NICI mode. A rapid and simple clean-up procedure of these drugs with use of Sep-Pak C18 cartridges is also presented. The drugs could be detected by gas chromatography with DB-1 and DB-17 capillary columns with satisfactory separation from impurities in their underivatized forms. The recovery of the drugs, which had been added to whole blood and urine, was more than 60% except for meclizine.

Authors+Show Affiliations

Department of Legal Medicine, Hamamatsu University School of Medicine, Japan.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

8307529

Citation

Seno, H, et al. "Positive- and Negative-ion Mass Spectrometry of Diphenylmethane Antihistaminics and Their Analogues and Rapid Clean-up of Them From Biological Samples." Forensic Science International, vol. 62, no. 3, 1993, pp. 187-208.
Seno H, Hattori H, Kumazawa T, et al. Positive- and negative-ion mass spectrometry of diphenylmethane antihistaminics and their analogues and rapid clean-up of them from biological samples. Forensic Sci Int. 1993;62(3):187-208.
Seno, H., Hattori, H., Kumazawa, T., & Suzuki, O. (1993). Positive- and negative-ion mass spectrometry of diphenylmethane antihistaminics and their analogues and rapid clean-up of them from biological samples. Forensic Science International, 62(3), 187-208.
Seno H, et al. Positive- and Negative-ion Mass Spectrometry of Diphenylmethane Antihistaminics and Their Analogues and Rapid Clean-up of Them From Biological Samples. Forensic Sci Int. 1993;62(3):187-208. PubMed PMID: 8307529.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Positive- and negative-ion mass spectrometry of diphenylmethane antihistaminics and their analogues and rapid clean-up of them from biological samples. AU - Seno,H, AU - Hattori,H, AU - Kumazawa,T, AU - Suzuki,O, PY - 1993/12/1/pubmed PY - 1993/12/1/medline PY - 1993/12/1/entrez SP - 187 EP - 208 JF - Forensic science international JO - Forensic Sci Int VL - 62 IS - 3 N2 - Positive-ion electron impact (PIEI), positive-ion chemical ionization (PICI) and negative-ion chemical ionization (NICI) mass spectra are presented for 15 compounds of diphenylmethane antihistaminics and their analogues, and each fragmentation pathway was analyzed. In the PIEI mode, molecular peaks were very small or missing for most compounds. Peaks at m/z 58, due to a dimethylaminomethyl group liberated, constituted base peaks in five compounds. Peaks at m/z 165 and/or 167, due to diaromatic rings plus a methyl group, appeared in most compounds. In the PICI mode, peaks due to M+H and M+C2H5 appeared in all compounds. Peaks due to diaromatic rings plus a methyl or ethyl group constituted base peaks in five compounds, which had an ether bond in their structures. In the NICI mode, anions at m/z M-H appeared in most compounds. Peaks at m/z 35 were observed for compounds having a chlorine group in their structures. Detection limits for total ion monitoring of these compounds were 20-50 ng on column in the PIEI mode, 100-200 ng in the PICI mode and 500-1000 ng in the NICI mode. A rapid and simple clean-up procedure of these drugs with use of Sep-Pak C18 cartridges is also presented. The drugs could be detected by gas chromatography with DB-1 and DB-17 capillary columns with satisfactory separation from impurities in their underivatized forms. The recovery of the drugs, which had been added to whole blood and urine, was more than 60% except for meclizine. SN - 0379-0738 UR - https://www.unboundmedicine.com/medline/citation/8307529/Positive__and_negative_ion_mass_spectrometry_of_diphenylmethane_antihistaminics_and_their_analogues_and_rapid_clean_up_of_them_from_biological_samples_ L2 - https://linkinghub.elsevier.com/retrieve/pii/0379-0738(93)90208-R DB - PRIME DP - Unbound Medicine ER -