title: Determination of Degradation Products of Cyclobenzaprine Hydrochloride, Lidocaine and Piroxicam in a Semi-Topical Formulation: MS-MS Confirmation of Unknown Impurities.
abstract: Association of cyclobenzaprine hydrochloride, piroxicam and lidocaine in a topical formulation is one of the newest innovations in the pharmaceutical formulary field. In this study, a reversed-phase liquid chromatographic method was developed for the establishment of the impurities of cyclobenzaprine hydrochloride, lidocaine and piroxicam in the semisolid topical formulation. In this study, we not only determined 2,6-dimethylaniline, 2-pyrydilamine but also specified impurities of cyclobenzaprine hydrochloride (dibenzosuberenone, amitriptyline, carbinole, cyclobenzaprine N-oxide and anthrachinone). The target compounds were determined using a mobile phase that consisted of a mixture of phosphate buffer (0.025 M; pH 6.2)-acetonitrile-methanol (60 : 13 : 27, v/v/v). A minimum of three supplementary possible degradation products were determined. Using mass spectrometry, the unspecified impurities were identified and the use of correlation matrices permitted the association with the possible source compounds. The chromatographic conditions were qualified and validated according to ICH guideline requirements to confirm specificity, linearity, accuracy and precision.
authors.affiliation: Department of Drug Analysis, University of Medicine and Pharmacy "Gr.T. Popa" Iasi, Universitatii Street, No. 16, Iaşi, Romania bogdan.cioroiu@gmail.com bogdan.cioroiu@chemperformance.ro.
authors.forename: Bogdan Ionel
authors.initials: BI
authors.lastname: Cioroiu
authors.affiliation: Department of Toxicology, University of Medicine and Pharmacy "Gr.T. Popa" Iasi, Universitatii Street, No. 16, Iaşi, Romania.
authors.forename: Ioana Cezara
authors.initials: IC
authors.lastname: Grigoriu
authors.affiliation: Department of Clinical Biochemistry, Clinical Hospital of Pulmonary Disease, Dr. I. Cihac Street, No. 30, Iaşi, Romania.
authors.forename: Mona Elisabeta
authors.initials: ME
authors.lastname: Cioroiu
authors.affiliation: Research Center for Oenology, Romanian Academy-Iasi Branch, Mihai Sadoveanu Street, No. 3, Iaşi, Romania.
authors.forename: Marius
authors.initials: M
authors.lastname: Niculaua
authors.affiliation: Fiterman Pharma, Pacurari Street, No. 127, Iaşi, Romania.
authors.forename: Roxana
authors.initials: R
authors.lastname: Lupuleasa
authors.affiliation: Department of Drug Analysis, University of Medicine and Pharmacy "Gr.T. Popa" Iasi, Universitatii Street, No. 16, Iaşi, Romania.
authors.forename: Mihai Ioan
authors.initials: MI
authors.lastname: Lazar
mesh_terms: D000639:Amitriptyline / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry; D008012:Lidocaine / Q000032:analysis / Q000737:chemistry*; D010894:Piroxicam / Q000032:analysis / Q000737:chemistry*; D053719:Tandem Mass Spectrometry
chemical_list: D010894:Piroxicam; D000639:Amitriptyline; C004704:cyclobenzaprine; D008012:Lidocaine