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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
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