Keywords: Pharmaceutical, Packaging, IV bags, intravenous delivery systems, Extractables, Leachables, Single Quad Mass Spectrometry, Time-of-Flight Mass Spectrometry, Stir Bar Sorptive Extraction (SBSE), Thermal Desorption, Thermal Extraction, Gas Chromatography
IV bag components were analyzed for extractables using direct thermal desorption/thermal extraction combined with a unit mass resolution GC/MSD system. The results were compared to those obtained for leachables by stir bar sorptive extraction of an aqueous simulant stored in the exact same type of IV bag, again combined with GC/MS determination of the leached compounds. In addition, the high resolution GC/Time of Flight (TOF) mass spectrometer was used to verify or disprove some of the MSD findings.
Keywords: Solid Phase Extraction, SPE, Liquid Chromatography, Sample Analysis, Lab Automation
Solid phase extraction (SPE) is one of the sample preparation methods most widely used by chromatographers, as demonstrated by the numerous published SPE methods found in the literature. Manual SPE cartridge formats can vary from disks through individual cartridges with a range of different volumes to 96-well plates. However, solid phase extraction methods can be tedious and time consuming when performed manually. There is therefore an increasing need for the automation of solid phase extraction methods. A robotic X-Y-Z coordinate autosampler commonly used for sample introduction in GC or HPLC can be used to perform a wide variety of sample preparation techniques using a single instrument and controlling software. The MAESTRO software allows the user to control the automation of solid phase extraction methods. In addition to ease of use and intuitive windows-based programming, the tools to optimize method parameters ensuring efficient sequence creation and maximum sample throughput. The sampler can be configured as part of a GC or LC system or as a benchtop workstation. In this study, we show that existing manual SPE methods can be transferred to standard format automation cartridges and automated using the robotic autosampler in conjunction with the software. Examples of solid phase extraction methods illustrating the conversion from manual to automated methods are shown.
Keywords: Static Headspace, Residual Solvents, USP <467>
USP Residual Solvents is a general chapter in the US Pharmacopeia that describes a headspace gas chromatographic method for the determination of residual solvents in pharmaceutical products, active ingredients, and excipients. As originally written, it described parameters used with balanced-pressure or pressure loop based headspace instruments. Recent updates have included parameters for syringe based systems.
This application note demonstrates implementation of USP Residual Solvents using the GERSTEL MPS configured as automated headspace sampler. Children’s non-aspirin (acetaminophen) suspension liquid was purchased locally and spiked to a level of 2000 μg/g (5 times the acceptable concentration limit) with acetonitrile.