Quantification of Gd species in a tetrameric Gd-based contrast agent using HPLC-ICP-MS

The scientific team of Dr. <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/articles?search=miloslav+polasek">Miloslav Polášek</a> at IOCB Prague has developed a new method of separating the rare earth elements, or lanthanides, which are widely used in the electronic, medical, automotive, and defense industries. The unique method allows metals such as neodymium or dysprosium to be purified from used neodymium magnets. The environmentally friendly process precipitates the rare earths from water without organic solvents or toxic substances. The results were published in the Journal of the American Chemical Society (JACS) at the end of June.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/IOCB_Prague_Tomas_Bellon_Dr_Miloslav_Polasek_head_of_the_Coordination_Chemistry_research_group_at_IOCB_Prague_and_Kelsea_Grace_Jones_Ph_D_student_in_Dr_Miloslav_Polasek_s_group_c94ff60915.jpg" alt="IOCB Prague / Tomáš Belloň: Dr. Miloslav Polášek, head of the Coordination Chemistry research group at IOCB Prague, and Kelsea Grace Jones, PhD student in Dr. Miloslav Polášek’s group. " srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_IOCB_Prague_Tomas_Bellon_Dr_Miloslav_Polasek_head_of_the_Coordination_Chemistry_research_group_at_IOCB_Prague_and_Kelsea_Grace_Jones_Ph_D_student_in_Dr_Miloslav_Polasek_s_group_c94ff60915.jpg 234w," sizes="100vw" width="1348" height="900">Global demand for rare earths is driven primarily by their use in extremely strong neodymium magnets, which enable efficient conversion of motion into electrical energy and vice versa. They are essential to manufacturers of electric cars, wind power plants, mobile phones, computers, and data centers. As these industries develop, demand for rare earths will continue to grow. However, the process of mining and purifying these elements is highly energy intensive and produces large amounts of toxic and radioactive waste.The rare-earth market is dominated by China, giving it leverage over Europe and North America. It is therefore strategically advantageous to focus on so-called urban mining, i.e. the recycling, renewal, and reuse of materials from discarded equipment, such as electric vehicles, as a significant domestic source of rare earths.“In the future, we won’t be able to cover the growing consumption of rare earths with primary mining. We know that within ten years at the latest, it will be necessary to manage these materials more carefully. In order to achieve this, the development of new technologies must start now,” explains Miloslav Polášek, head of the Coordination Chemistry group. “Our method solves the fundamental problems of recycling neodymium magnets. We can separate the right elements so that new magnets can be produced. Our process is environmentally friendly, and we believe that it will work on an industrial scale. Fortunately, unlike plastics, chemical elements don’t lose their properties through repeated processing, so their recycling is sustainable and can compensate for traditional mining.”<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/DSC_2799_2_d804034e7a.jpg" alt="IOCB Prague / Tomáš Belloň: A product of separation carried out using a method developed in Dr. Miloslav Polášek’s lab. He and his team processed a magnet from an electric car and obtained 99.7% pure neodymium." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_DSC_2799_2_d804034e7a.jpg 234w," sizes="100vw" width="1348" height="900">The topic, which Polášek’s group has been working on for a long time, is part of Kelsea G. Jones’s doctoral thesis. “We’ve developed a new type of chelator, which is a molecule that binds metal ions. This chelator specifically precipitates neodymium from dissolved magnets, while dysprosium remains in solution, and the elements are easily separated from each other. The method is also adaptable for the other rare earths found in neodymium magnets,” says Jones. “The separation is done in water and generates no hazardous waste. We achieve the same or better results than current industrial methods that rely on organic solvents and toxic reagents.”The new technology is patented and responds to a fundamental global problem at the right time. “We’re impatiently awaiting the results of a feasibility study, which will help us direct this research from the laboratory into practice. I believe that in cooperation with the investors and business partners we’re approaching, this new technology from IOCB Prague has the potential to influence a wide range of industrial sectors,” says Milan Prášil, director of the transfer company <a target="_blank" rel="noopener noreferrer" href="https://www.uochb.cz/en/iocb-tech">IOCB Tech</a>.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/DSC_0502_2_449fa66802.jpg" alt="IOCB Prague / Tomáš Belloň: Milan Prášil, director of the transfer company IOCB Tech." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_DSC_0502_2_449fa66802.jpg 234w," sizes="100vw" width="1348" height="900">This research has also yielded another important finding: namely, that the element holmium is used in neodymium magnets of newer electric cars. Scientists from Polášek's team discovered this by analyzing samples from the electric motors of European and Chinese cars. However, professional publications have not yet mentioned this fact, and most recycling projects do not take it into account when processing waste from electric cars. These findings will undoubtedly influence other development and recycling projects, even beyond the automotive industry.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/DSC_2816_2_80e809d242.jpg" alt="IOCB Prague / Tomáš Belloň: Kelsea Grace Jones, PhD student in Dr. Miloslav Polášek’s research group" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_DSC_2816_2_80e809d242.jpg 234w," sizes="100vw" width="1348" height="900"><blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/jacs.5c04150">Macrocyclic Chelators for Aqueous Lanthanide Separations via Precipitation: Toward Sustainable Recycling of Rare-Earths from NdFeB Magnets</a></h4>Kelsea G. Jones, Tomáš David, Martin Loula, Stanislava Matějková, Jan Blahut, Anatolij Filimoněnko, Miroslava Litecká, Jan Rohlíček, Jiří Böserle, Miloslav Polasek*J. Am. Chem. Soc. 2025<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/jacs.5c04150">https://doi.org/10.1021/jacs.5c04150</a><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/">CC-BY 4.0</a></h6></blockquote>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.<h4>Abstract</h4>Rare-earth elements (REEs) are critical materials in modern industry, but their production has a significant environmental footprint. Environmentally friendly separation methods would enable efficient, sustainable recycling of REEs. This work introduces a class of cyclen-based macrocyclic chelators that induce significant differences in solubility for REE chelates, enabling their selective precipitation from pH-neutral aqueous solution. The process was refined using simple coordinating additives (e.g., acetate) to form ternary coordination compounds to fine-tune these chelate solubilities. Conditions were optimized for the REEs found in NdFeB magnets, allowing separations of even adjacent lanthanides by repeated precipitations. Separation factors comparable to those of industrial solvent extraction methods were achieved without organic solvents. Analysis of NdFeB magnets from current electric car motors revealed an unexpected presence of holmium as a supplement and/or replacement for terbium and dysprosium, suggesting shifting industrial trends with implications for future recycling efforts. In a case study, one such automotive magnet was processed to obtain a 99.7% pure neodymium product. Scalable, tunable, and entirely aqueous, this approach advances the sustainable use of REEs toward a circular economy.<h4>Materials and Methods</h4>Liquid chromatography: Analytical HPLC experiments were performed on <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=1260+Infinity+II">1260 Infinity II </a>with UV (DAD, part number G7115A, 190 – 400 nm) and MS (single quadrupole, G6125B) detectors from Agilent (referred to as LC-MS or HPLC) equipped with a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1529">Luna Omega Polar C18 column</a> (5 µm, 100 Å, 150 × 4.6 mm) using H2O–MeCN gradients (1 mL min−1 flow rate) either with additives or without additives (specified where relevant). The UV-absorption profiles given for the characterization of the chelators and/or chelates were obtained from these chromatograms. Preparative HPLC experiments were performed on 1260 Infinity II (Agilent) equipped with YMC-Actus Triart C18 column (5 µm, 100 Å, 250 × 20.0 mm) using H2O–MeCN gradients (20 mL min−1 flow rate) with either TFA (0.1%) or no additional additive.High-resolution mass spectra: HRMS (with ESI ionization) were recorded on an Agilent 5975C MSD Quadrupole, <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?instrumentationItems=29-32&amp;manufacturerItems=5&amp;search=Q-Tof">Q-Tof micro</a> from Waters or <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=2&amp;search=LTQ+Orbitrap+XL">LTQ Orbitrap XL</a> from Thermo Fisher Scientific.Elemental analysis: CHN elemental analysis was performed on PE 2400 Series II CHN Analyzer from Perkin Elmer. Fluorine elemental analysis was performed by combustion of the sample in quartz vessel, followed by adsorption of HF in H2O and determining its concentration by potentiometry using F- -selective electrode. Lanthanide content was determined by ICP-OES (SPECTRO Arcos Multiview from SPECTRO Analytical Instruments). All EA data are presented as: calcd. (found).NMR spectroscopy: 1H and 13C NMR spectra were recorded on a Bruker Avance III™ HD 400 MHz spectrometer (401.0 MHz for 1H, 100.6 MHz for 13C) equipped with a broad-band Prodigy cryo-probe with ATM module (5 mm CPBBO BB-1 H/19F/D Z-GRD) or on an Avance II™ 500 MHz (Bruker, 499.9 MHz for 1H, 125.7 MHz for 13C) spectrometer equipped with a 5 mm TBO probehead. The measurement temperature is indicated for the respective chelator. Chemical shifts are in ppm and coupling constants in Hz. Spectra were referenced using the residual DMSO-d6 solvent signal (2.50 ppm in 1H; 39.52 ppm in 13C), or to the signal of t-BuOH external standard (1.25 ppm in 1H; 32.43 ppm in 13C) for spectra measured in D2O. Integrals in showcased NMR spectra were rounded to integers for clarity; obscured signals that cannot be exactly integrated due to overlap with peak from solvent are coloured grey. Signals of the cyclen macrocycle are abbreviated mc.X-ray powder diffraction: Data were acquired using the Debye-Scherrer transmission configuration on the powder diffractometer Smartlab (Rigaku) equipped with a Cu X-ray source (Cu/Kα radiation; λ = 1.5418 Å), focusing mirror (CBO-E), capillary holder and D/tex ultra 250 detector. The sample was ground, placed in a 0.5 mm borosilicate-glass capillary, and measured at 298±5 K over 18 h from 3° to 65° 2θ with 0.01° step size and with variable counting time.

A unique method of rare-earth recycling can strengthen the raw material independence of Europe and America

Professor Radek Cibulka's laboratory has long been trying to develop systems that would facilitate chemical reactions, and thus the ways how to easily synthesize some drugs or other useful substances. The prestigious journal Chemical Science has now published a new system for chemical reductions based on deprotonated flavins, derivatives of vitamin B2. The system was developed as part of a collaboration between teams from the University of Chemical Technology, Prague and Adam Mickiewicz University within LA project from Czech Science Foundation and National Science Centre (Poland). "We feel like builders. Removing one component (a proton) from a molecule of almost colourless 3-methyllumichrome - a substance related to flavins - causes structural changes that lead to the formation of an orange flavin anion. This flavin anion is unique because its protonated form does not exist. Moreover, we used this anion as a catalyst for reductions. All you have to do is shine cyan light on it and the reduction takes place." says Radek Cibulka.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.rsc.org/en/content/articlelanding/2025/sc/d5sc01630d">Introduction of flavin anions into photoredox catalysis: acid–base equilibria of lumichrome allow photoreductions with an anion of an elusive 10-unsubstituted isoalloxazine</a></h4>Dorota Prukała, Ekaterina Zubova, Eva Svobodová, Ludmila Šimková, Naisargi Varma, Josef Chudoba, Jiří Ludvík, Gotard Burdzinski, Iwona Gulaczyk, Marek Sikorski and &nbsp;Radek CibulkaChem. Sci., 2025,16, 11255-11263<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1039/D5SC01630D">https://doi.org/10.1039/D5SC01630D</a><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/3.0/">CC-BY 3.0</a></h6></blockquote>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.<h4>Abstract</h4>Flavins have been established as effective catalysts in oxidative photoredox catalysis. Conversely, their use in reductive photocatalysis remains limited, mainly due to the relatively low stability of the transient flavin radicals (semiquinones), which are used in photoreductions. The fully reduced forms of flavins are also disadvantaged in photocatalysis because they absorb light in the UV rather than in the visible region. In this work, we present a new approach for reductive flavin photocatalysis that utilises a flavin (isoalloxazine) anion derived from the elusive 10-unsubstituted 3,7,8-trimethylisoalloxazine, an unstable tautomer of 3-methyllumichrome. We found the conditions under which this isoalloxazine anion is formed by in situ deprotonation/isomerisation from the readily available 3-methyllumichrome and we subsequently used it as a photoredox catalyst in the reductive dehalogenation of activated bromoarenes and their C–P coupling reaction with trimethyl phosphite to form an arylphosphonate. Steady-state and transient absorption spectroscopy, NMR and cyclic voltammetry investigations, together with quantum chemical calculations, showed that the anion of oxidised isoalloxazine has several advantages, compared to other forms of flavins used in photoreductions, such as high stability, even in the presence of oxygen, an absorption maximum in the visible region, thereby allowing the use of excitation light between 470 and 505 nm, and a relatively long-lived singlet excited-state.<h4>Materials and methods</h4>Nuclear magnetic resonance (NMR) spectra were recorded in CD3CN, DMSOd6 , DMF-d6, TFA-d3 or in their mixtures on an Agilent 400-MR DDR2 (399.94 MHz for 1H, 100.58 MHz for 13C), JEOL-ECZL400G (400 MHz for 1H, 101 MHz for 13C), or Bruker Avance III 600 MHz (600 MHz for 1H and 151 MHz for 13C) at 298 K. Data for 1H NMR are reported as follows: chemical shift (δ ppm), multiplicity (s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet, dd = doublet of doublets, dt = doublet of triplets, br = broad etc.), coupling constant (Hz), and integration. All NMR spectra were processed and assigned using MestreNova. High-resolution mass spectra were obtained on <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=5&amp;search=Q-Tof+Micro">Q-Tof Micro</a> (Waters), equipped with a quadrupole and time-of-flight (TOF) analyser and a multichannel plate (MCP) detector. GC-MS analysis were performed on gas chromatograph <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=3&amp;search=Trace+GC+Ultra">Trace Ultra</a> (Themo Scientific) with a quadrupole mass spectrometer <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=3&amp;search=DSQ+II">DSQ II</a> (Thermo Scientific) equipped with DB-5ms capillary column (30 m x 0.25mm, film 0,25 um) or on gas chromatograph <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890">7890</a> (Agilent) with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/473">orbital trap mass spectrometer Exploris 240</a> (Thermo Scientific) equipped with DB-5ms capillary column (30 m x 0.25mm, film 0,25 um). <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=50&amp;search=SICRIT">SICRIT</a> (Soft Ionization by Chemical Reaction In Transfer - Plasmion GmbH, Germany) was used in positive mode. The melting points were measured on a Boetius melting point apparatus and are not corrected. Photoredox catalysis was performed using Luxeon Star LED 470 nm (65 lm @ 700mA) with dominant peak wavelengths 460–485 nm in tempered aluminium block (for arrangement, see S3) and Luxeon Star LED 505 nm (76 lm @ 350mA) with dominant peak wavelengths 490–515 nm. UV-Vis absorption spectra were recorded on a <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=UV-2550">UV-2550</a> spectrophotometer (Schimadzu). Steady-state emission spectra and fluorescence excitation spectra were recorded on a Jobin Yvon-SpexFluorolog 3-22 spectrofluorometer. Note that spectra were recorded using the same excitation and emission slits for uniform spectral resolution and sensitivity. Fluorescence lifetime measurements of all compounds were performed using the time-correlated single-photon counting (TCSPC) method. Decays were measured with the TCSPC Triple Illuminator as an accessory for the Fluorologs 3-22 steady-state spectrofluorometer that adds lifetime-capability in the time domain. The excitation source were NanoLED diodes (λexc = 368 nm and 389 nm) from IBH. The instrument in this hardware configuration is capable of measuring lifetimes as short as 400 ps. Deconvolution of fluorescence decay curves was performed using IBH Consultants software. The experimental uncertainties in the lifetimes are 10 %. Setup for UV-Vis transient absorption spectra measurements: The triplet states were generated and analysed using laser flash photolysis employing a nanosecond Q-switched Nd: YAG laser in combination with an optical parametric oscillator (OPO) operating at 470 nm; the laser pulse energy was kept around 0.5 mJ/pulse. The sample's solution was deoxygenated by bubbling argon for 15 min before measurements. Spectra were determined using kinetics collected between 350–700nm with a 10 nm interval. See ref.1 for details. Electrochemical measurements(cyclic voltammetry) were managed by a computer driven potentiostat <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=PGSTAT101">PGSTAT101 </a>(Autolab-Metrohm) using NOVA 1.11 software, for details see Chapter 5.

Work of Professor Cibulka's team featured on the cover of Chemical Science journal

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