Identification of the Impurities in Bopu Powder® and Sangrovit® by LC-MS Combined with a Screening Method

Bopu powder® and Sangrovit® were developed from Macleayacordata and are widely used in agriculture and animal husbandry, but their impurities have been rarely reported in the literature. Impurity analysis is of great importance to the quality and safety of veterinary drugs. In this study, high-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF-MS) combined with a screening method was used to screen and characterize the impurities in Bopu powder® and Sangrovit®. A total of 58 impurities were screened from Bopu powder® and Sangrovit® using the screening strategies, of which 39 were identified by their accurate m/z value, characteristic MS/MS data, and fragmentation pathways of references. This established method was used for impurity analysis for the first time and proved to be a useful and rapid tool to screen and identify the impurities of Bopu powder® and Sangrovit®, especially for those at trace levels in a complex sample. In addition, this study marks the first comprehensive research into impurities in these two products and has great significance for the systematic detection of impurities in other plant-derived drugs.

FTIR-based spectral line data of the v3 band of NO2 at 6.3 µm and multi-component impurity analysis of NO2 reference gases within the scope of the EMPIR MetNO2 project

<p>Air pollution causes hundreds of thousands of premature deaths every year in Europe [1]. Traffic related Nitrogen dioxide (NO<sub>2</sub>) is a key contributor whose concentration is legislated by the Ambient Air Quality Directive (EU, 2008) [2] and the air quality guidelines (AQGs) set by the World Health Organization (WHO). Atmospheric NO<sub>2</sub> concentration has been widely measured by national, regional and global monitoring networks using different instrumentations. SI-traceability is essential to assure data comparability across networks, underpinning long term trend of ambient NO<sub>2</sub>.</p><p>Traceable and accurate spectral line data [3,4] of NO<sub>2</sub> is essential for optical sensing of NO<sub>2 </sub>using in situ [5] and satellite-based equipment. In particular, it is essential for cost-effective light-weight systems with payload restrictions (e.g. TDLAS system [6], e.g. when installed on drones and balloons for which real time calibration using gas cylinders quickly becomes a burden). Within the scope of the EMPIR (The European Metrology Programme for Innovation and Research) MetNO<sub>2</sub> project [7], spectroscopic measurements of the selected NO<sub>2</sub> CRM (certified reference material) has been carried out using the FTIR infrastructure at PTB to a) derive traceable line data of NO<sub>2</sub>; b) quantify the amount of impurities, such as HNO<sub>3</sub>, N<sub>2</sub>O<sub>4</sub>, NO, N<sub>2</sub>O, CO, H<sub>2</sub>O, etc. Here, we report the line intensity and air-broadening coefficients of the 6.3µm v<sub>3</sub> band of NO<sub>2</sub>. FTIR-based impurity analysis including their temporal evolution will also be presented.</p><p><strong>Acknowledgement</strong></p><p>MK and GL thank for technical support from Kai-Oliver Krauss. This work has received funding from the EMPIR programme co-financed by the Participating States and from the European Union's Horizon 2020 research and innovation programme. PTB is member of the European Metrology Network for Climate and Ocean Observation (https://www.euramet.org/european-metrology-networks/climate-and-ocean-observation/).</p><p><strong>References</strong></p><p>[1] Air quality Europe – 2019 report.  EEA Report No 10/2019. https://www.eea.europa.eu/publications/air-quality-in-europe-2019</p><p>[2] Directive 2008/50/EC of the European Parliament and of the Council of 21 May 2008 on ambient air quality and cleaner air for Europe. https://www.eea.europa.eu/policy-documents/directive-2008-50-ec-of</p><p>[3] V. Werwein, J. Brunzendorf, G. Li, A. Serdyukov, O. Werhahn, V. Ebert.  Applied Optics 56 (2017)</p><p>[4] V. Werwein, G. Li, J. Brunzendorf, A. Serdyukov, O.Werhahn, V. Ebert. Journal of Molecular Spectroscopy 348, 68-78(2017).</p><p>[5] O. Werhahn O, J.C. Petersen (eds.) 2010 TILSAM technical protocol V1_2010-09-29. Available from:                     http://www.euramet.org/fileadmin/docs/projects/934_METCHEM_Interim_Report.pdf.”</p><p>[6] J. A. Nwaboh, Z. Qu, O. Werhahn and V. Ebert, Applied Optics 56, E84-E93 (2017)</p><p>[7] EMPIR project 16ENV02, “Metrology for Nitrogen Dioxide (MetNO<sub>2</sub>)”, http://em-pir.npl.co.uk/metno2/</p>