DOI: 10.5061/dryad.31zcrjdtj
title: Compendial testing data of bictegravir and cabotegravir

description: ISO/IEC 17043:2015, specifies general requirements for the competence of
 providers and development and operation of proficiency testing schemes. As
 a requirement of ISO/IEC 17043:2015 accreditation, the Clinical
 Pharmacology Quality Assurance Program uses ISO 17034 certified reference
 materials (CRMs) to produce proficiency testing materials. When CRMs that
 meet the ISO/IEC 17034 standard are not available or are prohibitively
 expensive, the purity and identity of non-certified standards must be
 authenticated by compendial testing to establish fit for intended use.
 Here, we report on a compendial testing approach used to assess whether
 standard reference materials for bictegravir and cabotegravir, two
 emerging drugs used in the treatment of HIV infection, are suitable for
 proficiency testing. Our approach uses high performance liquid
 chromatography and thermogravimetric analysis to evaluate purity of the
 materials and high-resolution mass spectrometry and proton nuclear
 magnetic resonance spectroscopy to establish molecular identity. Using
 this approach, we were able to certify standard reference materials for
 bictegravir and cabotegravir that are suitable for proficiency testing,
 providing some lower-costs alternatives.
description: HPLC experiments were conducted on a Shimadzu Prominence HPLC
 with PDA detection. Chromatograms were integrated and retention times,
 peak areas, and area percentages were recorded using the Shimadzu
 software. Thermogravimetric analysis has conducted on
 PerkinElmer TGA 8000. Sampling data was downloaded into a .csv file and
 processed in Microsoft Excel. High-resolution mass
 spectrometry analysis was conducted on a ThermoFisher Q Exactive Orbitrap
 mass spectrometer and the .RAW data files processed using
 XCalibur. Proton nuclear magnetic resonance analysis
 was conducted on a Bruker Avance NEO 400 MHz run with TopSpin software,
 and data were processed using the Mnova software from Mestrelab
 Research.
description: # Compendial testing data of bictegravir and cabotegravir
 [https://doi.org/10.5061/dryad.31zcrjdtj](https://doi.org/10.5061/dryad.31zcrjdtj) HPLC chromatograms of bictegravir and cabotegravir, including the calibration curves and purity analysis, is provided in two PowerPoint files named BIC HPLC purity chromatograms.pptx and CAB HPLC purity chromatograms.pptx, respectively. Excel files containing the raw data from thermogravimetry analysis, including plots of weight percentage vs. sample temperature, are provided in the following Excel files: TRCBICTGA.xlsx, CSBICTGA.xlsx, SigAmbeedCaboTGA.xlsx, TRCCaboTGA.xlsx, and CSCaboTGA.xlsx. High-resolution mass spectrometry data files are provided as .RAW files which can be processed by XCalibur: HRMS CS BIC.RAW, HRMS TRC BIC.RAW, HRMS TRC Cabo.RAW, HRMS CS Cabo.RAW, and HRMS SigmaAmbeed Cabo.RAW. Experimental NMR spectra were integrated and resonances determined using Mnova, and are depicted as .jpg files: NMR_Sigma_Cabo.jpg, NMR_TRC_Cabo.jpg, NMR_CS_Cabo.jpg, NMR_TRC_BIC.jpg, and NMR_CS_BIC.jpg. Simulated NMR spectra are provided as .png files: SimulatedProtonNMR_CAB.png and SimulatedProtonNMR_BIC.png. ## Description of the data and file structure The data include HPLC, thermogravimetry, high-resolution mass spectrometry, and proton nuclear magnetic resonance data from reference materials of bictegravir from Clearsynth and Toronto Research Chemicals, and of cabotegravir from Clearsynth, SigmaAmbeed, and Toronto Research Chemicals. Thermogravimetry and high-resolution mass spectrometry data is the actual raw data, whereas HPLC and NMR data are pictorial representations of the raw data. ## Sharing/Access information No special instructions. ## Code/Software XCalibur is required to read the .RAW high-resolution mass spectrometry data. Microsoft Excel is required to read the thermogravimetry data.