title: First derivative spectrofluorimetric determination of zopiclone and its degradation product, 2-amino-5-chloropyridine, in pharmaceutical formulations with preliminary tool in biological fluids for clinical evidence of zopiclone intake.
abstract: A simple, fast, sensitive and stability-indicating derivative spectrofluorimetric method is presented for the assay of zopiclone (ZOP), a drug with hypnotic effect, and its main degradation product and major contaminant, 2-amino-5-chloropyridine (ACP). The method is based on measuring the inherent fluorescence intensity of both drugs at λex=300nm in methanol, then differentiation using D1 (first derivative technique). The developed method was found to be rectilinear over a range of 0.2-4μg/mL of ZOP and 4-100ng/mL of ACP. The limits of detection were 0.05μg/mL of ZOP and 0.2ng/mL of ACP with the limit of quantitation of 0.17μg/mL of ZOP and 0.7ng/mL of ACP. The outcoming results of the proposed method were compared to those obtained by a reference method showing no significant statistical difference between them concerning precision and accuracy. Additionally, the developed method was applied for detecting ACP in spiked human urine and plasma specimens as a tool of clinical evidence of zopiclone intake that can be easily implemented in forensic laboratories. The proposed method was validated as per ICH guidelines.
authors.affiliation: Department of Chemistry, Faculty of Science, Al Faisaliah Campus, King Abdulaziz University, Jeddah 21533, Saudi Arabia.
authors.forename: Amirah S
authors.initials: AS
authors.lastname: Al-Attas
authors.affiliation: Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura 35516, Egypt. Electronic address: nasrjj@mans.edu.eg.
authors.forename: Jenny Jeehan
authors.initials: JJ
authors.lastname: Nasr
authors.affiliation: Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura 35516, Egypt.
authors.forename: Shereen
authors.initials: S
authors.lastname: Shalan
authors.affiliation: Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura 35516, Egypt.
authors.forename: Fathalla
authors.initials: F
authors.lastname: Belal
mesh_terms: D000328:Adult; D053961:Azabicyclo Compounds / Q000032:analysis* / Q000737:chemistry; D016903:Drug Monitoring; D004355:Drug Stability; D006801:Humans; D006863:Hydrogen-Ion Concentration; D057230:Limit of Detection; D016014:Linear Models; D008297:Male; D010879:Piperazines / Q000032:analysis* / Q000737:chemistry; D011725:Pyridines / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D013050:Spectrometry, Fluorescence / Q000379:methods*; D055815:Young Adult
chemical_list: D053961:Azabicyclo Compounds; D010879:Piperazines; D011725:Pyridines; C515050:zopiclone; C108972:2-amino-5-chloropyridine
keywords: Biological fluids; Drug monitoring; Spectrofluorimetry; Stability-indicating; Zopiclone