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Analytical method for detection and quantification of new emerging drug etaqualone in human blood and urine by gas chromatography tandem mass spectrometry
Institution:1. Department of Forensic Analytical Toxicology, West China School of Basic Science and Forensic Medicine, Sichuan University, Chengdu, China;2. Department of Legal Medicine, College of Basic Medical Sciences, Inner Mongolia Medical University, Hohhot, China;1. Forensic DNA Typing Laboratory, Centre of Excellence in Molecular Biology, University of the Punjab Lahore 53700, Pakistan;2. Faculty of Life Sciences and Informatics, Balochistan University of Information Technology, Engineering and Management Sciences, Quetta (BAUITEMS), Pakistan;1. Department of Forensic Medicine and Toxicology, All India Institute of Medical Sciences, Jodhpur 342005, India;2. School of Forensic Sciences, National Forensic Sciences University, Tripura 799001, India;3. Department of Diagnostic and Interventional Radiology, All India Institute of Medical Sciences, Jodhpur 342005, India;4. Department of Anatomy, All India Institute of Medical Sciences, Jodhpur 342005, India;5. Department of Anthropology, (UGC Centre of Advanced Study), Panjab University, Chandigarh 160014, India;1. Department of Ophthalmology, Dr. Rajendra Prasad Centre for Ophthalmic Sciences, All India Institute of Medical Sciences, New Delhi, India;2. Department of Forensic Medicine and Toxicology, All India Institute of Medical Sciences, New Delhi, India;3. Department of Ocular Pharmacology and Pharmacy, Dr. Rajendra Prasad Centre for Ophthalmic Sciences, All India Institute of Medical Sciences, New Delhi, India
Abstract:Analytical procedure for detection and quantification of etaqualone in human blood and urine using GC–MS/MS was established and applied to authentic human samples obtained from volunteers. A liquid–liquid extraction method was employed. Each 1.0 mL of blood or urine was alkalized and extracted with diethyl ether. The solvent layer was evaporated to dryness and reconstituted with methanol then analyzed by GC–MS/MS. linear relationships within the concentration range of 1–100 ng/mL were obtained in calibrators for both blood and urine, demonstrating correlation coefficients values being>0.999. For blood and urine samples, the intra-day assay precision and accuracy values are each less than 3.65%, 7.13%, and 6.02%, 9.12%; those values of the inter-day assay are each less than 1.82%, 6.74%, and 3.99%, 7.41%. The extraction recovery rates for etaqualone ranged from 98.7% to 106%. The lower limit of quantifications was 1.0 ng/mL in both blood and urine. Stabilities of etaqualone in blood and urine were satisfactory under various temperatures within 15 days. 8.51 and 2.06 ng/mL of etaqualone in blood and urine were detected at 4 h later oral ingestion; 6.91 and 3.94 ng/mL of etaqualone were also detected 30 min and 2 h later smoking from blood and urine.
Keywords:Etaqualone  Excretion  Human samples  Internal standard method  GC–MS/MS
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