title: Simultaneous determination of zopiclone and its degradation product and main impurity (2-amino-5-chloropyridine) by micellar liquid chromatography with time-programmed fluorescence detection: preliminary investigation for biological monitoring.
abstract: A simple and reliable HPLC method was developed and validated for the simultaneous determination of the hypnotic drug, zopiclone (ZPC) and its degradation product and main impurity, 2-amino-5-chloropyridine (ACP). The analyses were carried out on BDS Hypersil phenyl column (4.6 mm × 250 mm, 5 μm particle size) using micellar mobile phase consisting of 0.15M SDS, 10% n-propanol, 0.3% triethylamine, and 0.02 M orthophosphoric acid (pH 3.5) with timed programmable fluorescence detection. The proposed method was found to be rectilinear over the concentration ranges of 0.5-10.0 μg/mL for ZPC and 2.5-50 ng/mL for ACP. Moreover, the method was applied for the determination of ZPC in commercial tablets with mean percentage recovery of 99.06±1.49. The results of the proposed method were statistically compared with those obtained by the comparison method revealing no significance differences in the performance of the two methods regarding accuracy and precision. Furthermore, the proposed method was applied for the detection and determination of ACP in human urine as a marker for ZPC intake.
authors.affiliation: Analytical Chemistry Department, Faculty of Pharmacy, Mansoura University, 35516 Mansoura, Egypt. rania_n2010@yahoo.com
authors.forename: R N
authors.initials: RN
authors.lastname: El-Shaheny
authors.forename: A
authors.initials: A
authors.lastname: Alattas
authors.forename: J J
authors.initials: JJ
authors.lastname: Nasr
authors.forename: N
authors.initials: N
authors.lastname: El-Enany
authors.forename: F
authors.initials: F
authors.lastname: Belal
mesh_terms: D000433:1-Propanol / Q000737:chemistry; D000328:Adult; D053961:Azabicyclo Compounds / Q000737:chemistry / Q000652:urine*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004340:Drug Contamination; D004355:Drug Stability; D005260:Female; D006801:Humans; D006863:Hydrogen-Ion Concentration; D016014:Linear Models; D008823:Micelles; D010879:Piperazines / Q000737:chemistry / Q000652:urine*; D011725:Pyridines / Q000737:chemistry / Q000652:urine*; D015203:Reproducibility of Results; D012967:Sodium Dodecyl Sulfate / Q000737:chemistry; D013050:Spectrometry, Fluorescence / Q000379:methods*; D013607:Tablets / Q000737:chemistry; D013696:Temperature
chemical_list: D053961:Azabicyclo Compounds; D008823:Micelles; D010879:Piperazines; D011725:Pyridines; D013607:Tablets; C515050:zopiclone; C108972:2-amino-5-chloropyridine; D012967:Sodium Dodecyl Sulfate; D000433:1-Propanol