We think you have liked this presentation. If you wish to download it, please recommend it to your friends in any social system. Share buttons are a little bit lower. Thank you!
Presentation is loading. Please wait.
Published byMatthew Rollins
Modified over 2 years ago
Materials Austin Pharma API, Dronabinol, USP Capsules manufactured from Austin Pharma API Marinol ® (RLD) Generic Dronabinol manufactured by Par Pharmaceuticals Methods HPLC method conditions are based on USP 29 monograph for Dronabinol. LCMS run conditions were adapted from the HPLC method using ammonium formate as the mobile phase additive for MS detection. Capsules were extracted based on USP Dronabinol capsule monograph. Materials and Methods Tetrahydrocannabinol ( 9 -THC) is a psychoactive substance found in cannabis plants (Medical Marijuana). Synthetic 9 -THC, also called Dronabinol, was approved by US FDA as a drug to treat pain, anorexia and nausea related to chemotherapy and other disorders. Dronabinol is a light yellow to amber glassy material. It is sensitive to light, heat, and oxygen (air). The impurities in commercial Dronabinol drugs may come from either the synthetic process or through product degradation. Identification of these impurities is required by FDA and ICH guidelines for pharmaceuticals. A comparison of impurities in Dronabinol from a variety of sources was performed by HPLC and LCMS. Authors: Huahua Jian, Isil Dilek, Uma Sreenivasan, Kenan Yaser Investigation of the Impurities in Dronabinol Samples by LC/MS Instrument Agilent G6410 Series Triple Quad (QQQ) LC/MS/MS Column Phenomenex Luna 3u C18(2) 150x4.6 mm Column Temperature20ºC Mobile Phase 71:24:5 v./v. MeOH/H 2 O/THF, with 5 mM ammonium formate GradientIsocratic Flow Rate1 mL/min Injection Volume5-20 µL UV wavelength228 nm Polarity, scan typePositive scan Ionization SourceElectrospray Ionizaion (ESI) Mass scan range Da RRTm/zM.W. Generic Brand Capsule Made from AustinPharm a API Marinol® Par Generic Austin Pharma API Sample Stressed API Sample Enriched with Impurities Identification , a+Hydroxydihydrocannabinol Trihydroxydihydrocannabinol Dihydroxydihydrocannabinol , a +, aHydroxydihydrocannabinol Hydroxydihydrocannabinol , aDihydroxydihydrocannabinol Dihydroxydihydrocannabinol Cannabidiol Hydroxycannabinol Dihydrocannabinol Hydroxydihydrocannabinol Dihydrocannabinol b++Cannabinol , b + Dihydrocannabinol Cis 9 -THC NA Dronabinol, API Dihydrocannabinol , a+Dihydrocannabinol THC Dronabinol Chromatogram s HPLC Chromatogram: TIC Chromatogram: Comparison of Impurity Profiles of Dronabinol Mass Spectra of Selected Impurities Structures of Dronabinol Impurities Identification of the specified impurities were confirmed by comparison to authentic references: RRT 0.78 – Cannabinol; RRT Cis 9 -THC; RRT THC. The proposed structures of other impurities were based on LCMS results. Extracted Ion Chromatogram (EIC) confirmed the relative retention time of these impurities. MRM studies did not provide additional information as the impurities are similar in structure. Impurities in Dronabinol Samples were identified. Specified impurities were Cannabinol, cis- 9 -THC and 8 -THC. Unspecified impurities were typically oxidative in nature. Structures were proposed for the observed unspecified impurities based on LCMS results. Similar impurity profiles were observed in all three capsules and stressed API, with an increase in number and amount of impurities. Conclusions © 2010 Cerilliant Corporation | 811 Paloma Drive | Round Rock, TX : Present in sample. : Not detected in sample or peak is too small to be extracted. a: Mass spectrum is compromised because the impurity is low in the sample. b:The mass spectra of RRT 0.82 for fresh API sample is 312. For the other four samples, it is a mixture of two components, with molecular weights 312 and 328. The ratio of the two peaks varies, but m/z 313 (M+H+) and m/z 329 (M+16+H+) are all evident. The m/z 329 peaks is oxygen adduct of m/z 313 peak. The structure of this impurity is proposed to be an isomer of Dihydrocannabinol and its oxygen adduct. Introductio n RRT 0.30 – Hydroxydihydrocannabinol RRT Cannabinol RRT Cis 9 -THC RRT 1.06 – Dihydrocannabinol
A practical approach to metabolomics Rob Linforth Food Sciences – Biosciences University of Nottingham.
Analytical Method Development and Validation Bob Seevers.
LC – MS Liquid chromatography coupled with Mass spectroscopy by Karnaker Reddy.T M.pharmacy.
Guilin, January, 9 – 13, 2006 Dr. Birgit Schmauser, BfArM, Bonn Verification of applicability of the validated/compendial API analytical method for the.
Syagen Technology, Inc Warner Avenue Tustin, CA APPI-LC/MS Analysis of Acylglycerols Sheng-Suan Cai, Luke Short, and Jack Syage.
1 Gas Chromatography There an be many parts to a gas chromatography system but the basic components include: An injection system. A column (controllable.
We then examined the interactions of Diuron, Diazinon, Alachlor and dEHP with both ODNs. The studied sequences are self-complementary and capable of assembling.
Lynda Paleshnuik | January |1 | Quality Workshop Copenhagen – January 2012 Assessing specifications: FPP (solid orals)
Why Mass Spectrometry: An Introduction to the IU MSF Jonathan A. Karty, Ph.D.
GAS CHROMATOGRAPHY. Classification based on Mobile Phase Gas Chromatography Gas - solid Gas - liquid Stationary Phase Sample MUST be volatile at temperatures.
The world leader in serving science PLOT GC Columns and Applications Bonded TracePLOT Columns.
Mass Spectrometry. Used to identify organic compounds mainly through molar mass and identification of major fragments. A mass spectrometer is often.
Process Analytical Technologies Process and Method Validation February 2002 FDA Subcommittee Meeting Leon Lachman, Ph.D. President Lachman Consultant Services,
1 Chemical Analysis by Mass Spectrometry Dr Phil Mortimer Chemistry Department Mass Spectrometry Facility
Option B – Medicine and Drugs IB Chemistry. 2 Pharmaceutical Products >A drug or medicine is any chemical which: Alters sensory sensations Alters mood.
Quality Control in Forensic Toxicology and Doping Analysis TIAFT Laboratory Guidelines Rudhard Klaus Mueller Institute of Doping Analysis Dresden and Leipzig.
ENVE 202 Dr. Aslıhan Kerç GAS CHROMATOGRAPHY. Gas Chromatography (GC) *Gas chromatography is a chromatographic technique that can be used to separate.
GC and GC-MS. Gas Chromatography Function Components Common uses Chromatographic resolution Sensitivity.
6 th Annual Science and Standards Symposium January 16, 2013 Istanbul Quality Attributes for Biological Medicines and USP Standards Fouad Atouf, Ph.D.
INDUSTRIAL HYGIENE DIRECT-READING INSTRUMENTS FOR GASES, VAPORS, AND PARTICULATES UNIVERSITY OF HOUSTON - DOWNTOWN.
R.Lo Curto, F. Vilasi, T. M. Pellicanò, P.Munafò, G. Dugo PRESENCE OF OCHRATOXIN A IN EXPERIMENTAL WINES RELATED TO CHEMICAL AND NATURAL TREATMENTS EMPLOYED.
Laser Ablation of Silicone Composites I. L. Hosier 1*, M. S. Abd Rahman 1, A. S. Vaughan 1, A. Krivda 2, X. Kornmann 2, L. E. Schmitt 2 1 University of.
1 RP HPLC Purification of Small Molecules Lou Cheng Astrazeneca R&D Boston.
EDQM Certification scheme: Common deficiencies observed in new chemical applications Dr P.Poukens-Renwart Certification of Substances Division, EDQM &
Structural characterization begins with a purity check! Elemental Analysis (EA) Thin Layer Chromatography (TLC) High Performance Liquid Chromatography.
1 Section 8.2 Determining Absolute Age. Objectives Summarize the limitations of using the rates of erosion and deposition to determine the absolute age.
1 Chapter 15: Two-Factor Analysis of Variance. 2 Two-Factor Designs In the context of ANOVA, an independent variable (or a quasi-independent variable)
1 of 30© Boardworks Ltd of 30© Boardworks Ltd 2007.
New 1100 Series DAD SL and MWD SL 80Hz Data Acquisition for Ultra-fast LC.
A Comprehensive Mössbauer Study of the Iron Uptake Strategies in Plants K. Kovács 1, E. Kuzmann 1, F. Fodor 2, A. Vértes 1 1 Laboratory of Nuclear Chemistry,
© 2016 SlidePlayer.com Inc. All rights reserved.