Ion Source Research Articles

Real-time analysis of anodic mixed gas generated on carbon electrodes during TiO reduction in a LiCl-based salt at 650 °C

The anode gas components produced during the electrolytic reduction of TiO was analyzed in this study in real time using a carbon anode in LiCl containing various Li2O and Li2CO3 concentrations under high-potential operation at 650 °C. A molten salt with 0.3 wt.% Li2O under 6 V cell voltage predominantly generated CO2 until depletion of the initial oxygen ion source, after which Cl2 gas began to form. A molten salt containing 0.2 and 1.3 wt.% Li2O and 1.3 wt.% Li2CO3, respectively, also generated CO2 as the main anode gas, followed by CO, O2, and Cl2 gas generation. In contrast, a molten salt with 0.8 and 0.5 wt.% Li2O and Li2CO3, respectively, initially generated CO, leading to carbonate accumulation, which gradually decreased as the concentration of generated CO2 increased and it became the dominant gas, while that of O2 remained constant (6–9%). Cl2 was predominantly generated upon depletion of the oxygen ion source in the salt. Cl2 reacted with carbonate ions in the salt, thus releasing CO2 gas and preventing carbonate accumulation in the salt. This study revealed that anode gas composition during electrolytic reduction with carbon anodes is critically influenced by the oxygen ion source concentration of the salt.

Development of a high-yield compact D-D neutron generator

An improved high-yield compact D-D neutron generator has been developed for active neutron non-destructive interrogation at Lanzhou University in China. The generator has been meticulously designed based on the magnetic field distribution of the duoplasmatron ion source, the electric field distribution of the beam extraction acceleration system, beam transport, and target cooling system. The performance characteristics of the generator were measured under different deuterium beam energies and beam intensities. The experimental results indicated that the D-D neutron yield reached 1×109 n/s with the deuterium beam parameter of 210 keV/6.0 mA. The operational stability of the generator was assessed for 150 minutes, and the test results show that the generator has better stability in operation. This generator has potential applications in neutron radiography, active interrogation of special nuclear materials, and neutron activation analysis.

An ion soft-landing apparatus for ion transport study with surface potential measurement.

An apparatus for explorations of ion transport in a medium and across an interface has been constructed. The ion soft-landing technique is used to deposit low-energy ions onto a pre-adsorbed medium layer on a metal substrate. The designed low-energy ion source can produce a mass-filtered ion beam with tens of nanoampere from solid sources such as bulk metals and salts. The kinetic energy of the ion beam can be lower than 1.0eV, enabling the ions to be soft-landed onto the medium at the surface. A Kelvin probe with a resolution of less than 32 mV is incorporated to measure the surface potential (SP) variation of the ion-landed sample to monitor the ion transport process in the medium. Temperature-programmed SP measurements on an Ag+-adsorbed ice film prepared on Pt(111) reveal that the temperature threshold for the Ag+-induced SP change of the ice film is about 110K. The apparatus performance demonstrates its potential in studies of ion transport and related phenomena at both macroscopic and microscopic levels.

TBAPy-based metal-organic frameworks with phosphate-induced fluorescence for detecting gossypol

How to achieve good dispersion of MOFs (metal–organic frameworks) is the key to its application in many fields. In our work, a novel MOF nanocomposite TBAPy-Yb was synthesized by solvothermal approach with TBAPy [1,3,6,8-tetrakis(p-benzoic acid)pyrene)] as the organic ligand and lanthanide metal ions as the metal ion source. Due to the coordination between phosphate and TBAPy-Yb, TBAPy-Yb had excellent dispersion in phosphate buffer and induced strong fluorescence emission in 435 nm. Gsp (gossypol) could regularly and instantly quench the induced fluorescence of TBAPy-Yb in the range of 10.0 to 70.0 μM and cause an obvious color change from blue to colorless. The detection limit was as low as 4.57 μM. The possible interferences in cottonseed oil did not influence the detection. The proposed method was effectively applied toanalyzeGsp oil with a recovery rate ranging from 94.20 % to 104.90 %. Furthermore, a portable and smart sensing platform was developed based on probe fixation and mobile phones.

Inferring ion cluster lifetimes from energy-resolved mass spectra of an EMI-BF4 electrospray plume

The fragmentation of ion clusters within the accelerating fields of ionic liquid ion sources (ILISs) is well documented and degrades ILIS performance and lifetime. Some of the most popular ILIS liquids, such as EMI-BF4 (1-Ethyl-3-methylimidazolium tetrafluoroborate) and EMI-Im (1-Ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide), emit clusters with lifetimes as low as ∼1 ns. Studies of fragmentation within the accelerating field typically rely on measuring the plume energy distribution averaged over all plume species and comparing those measurements with numerical simulations to estimate ion cluster lifetimes. Here, for the first time, we estimate EMI-BF4 cluster lifetimes by analyzing the energy distributions of individual plume species. We use this novel analysis method to estimate mean lifetimes of positive EMI-BF4 ion clusters from previously published experimental data. We find that the mean lifetime ranges from τ=3.7ns to τ=124ns for [EMI+][EMI-BF4] dimers and ranges from τ=1.5ns to τ=23ns for [EMI+][EMI-BF4]2 trimers. Fitting those data to an analytical fragmentation model, we estimate the binding energy and temperature as ΔGS0=0.49eV and T=394K for dimers and ΔGS0=0.40eV and T=365K for trimers. Comparing our results with previous studies supports the conclusion that clusters are emitted with a wide distribution of internal energies, contrary to the common assumption of single internal energy for each species.

UPLC-MS/MS analysis of axitinib and pharmacokinetic application in beagle dogs

ObjectiveTo develop a method for determining the concentration of axitinib in beagle dog plasma and utilize this method to investigate the pharmacokinetics of orally administered axitinib in beagle dogs. MethodsPlasma samples were processed using acetonitrile precipitation and analyzed by UPLC-MS/MS with sunitinib as an internal standard (IS). Chromatographic separation was achieved on a Waters Acquisition UPLC BEH C18 column (50 mm × 2.1 mm, 1.7 μm) with a gradient elution of acetonitrile and 0.1 % formic acid. Mass spectrometry uses an electrospray ion source for positive ion detection in a multiple reaction monitoring mode. The monitored ion transitions for axitinib and sunitinib were m/z 387 → 355.96 and m/z 399.3 → 282.96, respectively. Six beagle dogs were administered 0.33 mg/kg of axitinib orally, and venous blood samples were collected at 0.5, 1, 1.5, 2, 3, 4, 6, 8, 12, and 24 h post-dose for pharmacokinetic analysis. ResultsThe assay demonstrated a linear range of 0.5–100 ng/mL (r2 = 0.9992), and the lower limit of quantification was up to 0.5 ng/mL. Precision, as assessed by relative standard deviation (RSD), was within 8.64 % for both intraday and interday variability. The relative error (RE) for precision from −2.77 %–1.20 %. The recovery rate of the analytes exceeded 85.28 % and the matrix effect was approximately 100 %. Plasma samples maintained stability under various conditions, including room temperature storage for 12 h, processed on an automatic sampler at 4 °C for 6 h, three freeze-thaw cycles, and long-term storage at −80 °C for 60 days. Pharmacokinetic parameters were determined using DAS 2.0 software, revealing a half-life (T1/2) of 6.05 h and an area under the curve (AUC (0 →∞)) of 97.13 ng h/mL for axitinib. ConclusionsThe UPLC-MS/MS method developed in this study offers high specificity, rapid analysis, high recovery, excellent linearity, and minimal plasma volume requirements, making it well-suited for pharmacokinetic and drug interaction studies in beagles dogs.

Active Galactic Nuclei in the Green Valley at z ∼ 0.7

We present near-infrared (NIR) spectroscopy using the MMT and Magellan infrared spectrograph for a sample of 29 massive galaxies ( logM*/M⊙≳10 ) at z ∼ 0.7 with optical spectroscopy from the Large Early Galaxy Astrophysics Census (LEGA-C) survey. Having both optical and NIR spectroscopy at this redshift allows us to measure the full suite of rest-optical strong emission lines, enabling the study of ionization sources and the rest-optical selection of active galactic nuclei (AGN), as well as the measurement of dust-corrected Hα-based star formation rates (SFRs). We find that 11 out of 29 galaxies host AGN. We infer the nonparametric star formation histories with the spectral energy distribution fitting code Prospector and classify galaxies as star-forming, green valley, or quiescent based on their most recent specific SFRs. We explore the connection between AGN activity and suppressed star formation, and find that 89% ± 15% of galaxies in the green valley or below host AGN, while only 15% ± 8% of galaxies above the green valley host AGN. We construct the star-forming main sequence (SFMS) and find that the AGN host galaxies are 0.37 dex below the SFMS, while galaxies without detectable AGN are consistent with being on the SFMS. However, when compared to a bootstrapped mass-matched sample, the SFRs of our sample of AGN host galaxies are consistent with the full LEGA-C sample. Based on this mass-matched analysis, we cannot rule out that this suppression of star formation is driven by other processes associated with the higher mass of the AGN sample. We therefore cannot link the presence of AGN activity to the quenching of star formation.

Substrate modification for high performance CrAl/CrAlBN multilayers coated TiCN-based cermet through plasma nitriding

The plasma nitriding process was conducted on a TiCN-based cermet that had been coated with a multilayer CrAl/CrAlBN coating deposited via cathodic arc. The intensity of the plasma nitriding was modified by adjusting the anode current of the ionization source. To investigate the interface conditions, techniques such as electron probe X-ray microanalysis, electron backscatter diffraction, and transmission electron microscopy were employed. The results indicated that increasing the anode current led to the formation of a thicker nitrided layer and an increase in the texture coefficient of the (111) plane. Specifically, at an anode current of 200 A, the lattice mismatch degree at the TiCN/CrAlN interface decreased from 16.4 % to 3.7 %, resulting in the formation of a nearly coherent interface. The hardness, adhesion strength, and H/E ratio of the coating reached their peak values, and the coated cutting tool exhibited optimal cutting performance when machining the GH4149 superalloy.

Pharmacokinetic and tissue distribution study of pectolinarigenin in rats using UPLC-MS/MS

Pectolinarigenin (PEC), a natural flavonoid isolated from Cirsium japonicum, exhibits promising therapeutic potential for multiple cancers. In present study, a simple and sensitive UPLC-MS/MS method was established for the quantification of PEC in rat plasma and tissues. The assay procedure involved a one-step protein precipitation with tadalafil as the internal standard, and separation on a Welch Xtimate UHPLC C18 column by gradient elution of acetonitrile/aqueous formic acid (0.1 %, v/v) at a flow rate of 0.2 m L·min−1. The detection was conducted using multiple-reaction monitoring via an electrospray ionization source in positive ionization mode. The established method was proved to be highly sensitive with a good linearity (R2 > 0.99) in respective concentration range (0.1–100 ng·mL−1 in plasma and 1–10000 ng·mL−1 in tissues) and acceptable extraction recovery (≥71.17 %), matrix effect and stability, which was applied to study the pharmacokinetics and tissue distribution of PEC after intravenous (100 μg·kg−1) and oral administration (10, 20 and 40 mg·kg−1). PEC was promptly absorbed (Tmax ≤ 0.222 h) and maintained at a low level with slow elimination (t1/2 z ≥ 14.47 h) in rats after oral administration, resulting in extremely low bioavailability (0.56–0.68 %). However, PEC is widely distributed in rat tissues with high exposure in GI tract, liver and kidney. The bioavailability and tissue affinity were firstly revealed, which will guide directions for further development of PEC as an anti-tumor drug candidate.

Determination of deoxynivalenol and metabolites in maize samples by LC-MS/MS

In Vietnam, the regulation QCVN 8-1:2011/BYT has been issued to control mycotoxin content in food products. However, there are currently no regulations or studies on their derivatives and metabolites. Deoxynivalenol-3-glucoside (D3G) and two acetylated derivatives of deoxynivalenol (DON), namely 15-acetyldeoxynivalenol (15-AcDON) and 3- acetyldeoxynivalenol (3-AcDON), have been frequently detected in naturally contaminated grains such as wheat, barley, and corn. This study developed and applied a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to determine deoxynivalenol (DON) and its metabolites, including deoxynivalenol-3-glucoside (D3G), 3- acetyldeoxynivalenol (3-AcDON), and 15-acetyldeoxynivalenol (15-AcDON) in maize. The instrumental conditions comprised a C18 HSS SB (150 mm × 2.1 mm × 1.7 µm) column for separation and an MS/MS detector in positive and negative electrospray ionization (ESI) source, employing multi-reactive ion monitoring mode, with an injection volume of 2 µL. The method has been fully validated and meets the performance requirements of AOAC, demonstrating high specificity. The linearity range was established from 100 µg/kg to 1000 µg/kg, with a method detection limit (MDL) of 30 µg/kg. The repeatability and recovery rates were determined to be between 1.45% to 4.31% and 90% to 110%, respectively. The validated method was applied to analyze 50 maize samples. Deoxynivalenol (DON) was detected in 10 samples (20%), while deoxynivalenol-3-glucoside (D3G), 3- acetyldeoxynivalenol (3-AcDON), and 15-acetyldeoxynivalenol (15-AcDON) were not detected in any of the samples.

On the analytical soliton approximations to damping forced Zakharov-Kuznetsov equation arising in dissipative nonthermal magnetized plasma

Abstract This paper aims to analyse the nonlinear characteristics of ion-acoustic solitary waves (IASWs) in a plasma system that is collisional and homogeneous in nature. The system under consideration comprises positive ions, negative ions, and nonthermal electrons and is influenced by an ambient magnetic field. To analyse the system, we utilize the reductive perturbation technique (RPT) and obtain the damped forced Zakharov-Kuznetsov (DFZK) equation. The DFZK equation provides a solitary wave solution when an external periodic force is present. Through numerical analysis of DFZK, we have observed that different parameters, e.g., the nonthermal parameters (r,q), the direction cosine, the temperature ratio of a positive ion to an electron, the temperature ratio of a negative ion to an electron, the density ratio of a negative ion to a positive ion source strength, and the source frequency, affect the phase velocity and the structures of IASWs significantly. This finding could help clarify the plasmas observed in the D- and F-regions of Earth's ionosphere, as well as in laboratory experiments where pair ions and nonthermal electrons are key characteristics.

Determination of some NSAIDs content in meat by liquid chromatography with tandem mass spectrometry (LC-MS/MS)

Nonsteroidal anti-inflammatory drugs (NSAIDs) are the most widely used group of drugs worldwide for pain relief, anti-inflammation, blood clot prevention, and fever reduction, but they can cause some side effects bad for health if used incorrectly. NSAIDs are on the list of drugs that must be monitored according to Council Directive 96/23/EC. The fact that NSAIDs are also used in animals for anti-inflammation, fever reduction, and pain relief raises concerns that animal products such as meat, eggs, and milk may be contaminated with NSAIDs, affecting human health if consumed like eating right. Therefore, developing a method to analyze NSAIDs in meat products is necessary, contributing to assessing the quality of meat products currently circulating on the market. In this study, 4 common substances in the NSAIDs group were studied and identified by liquid chromatography with tandem mass spectrometry (LC-MS/MS) using a Symmetry C18 chromatographic column with an ESI (+) positive electron spray ionization source and multiple reaction monitoring (MRM) mode. The validity of the method was confirmed according to the guidelines of the Association of Official Analytical Chemists (AOAC). The results showed that the method has good specificity, the linearity range from 5.0 to 100 µg/kg, the detection limit of 1.5 µg/kg, the quantification limit of 5.0 µg/kg; precision and accuracy with relative standard deviation (RSD) less than 11% and recoveries ranging from 81.1 to 111%, meeting AOAC requirements. The method was used to analyze the content of NSAIDs in 15 meat samples in Hanoi. The results showed that 7 samples showed tolfenamic acid exceeding the quantitative limit of the method.

Microbial Metabolomics' Latest SICRIT: Soft Ionization by Chemical Reaction In-Transfer Mass Spectrometry.

Microbial metabolomics studies are a common approach for identifying microbial strains that have a capacity to produce new chemistries both in vitro and in situ. A limitation to applying microbial metabolomics to the discovery of new chemical entities is the rediscovery of known compounds, or "known unknowns." One factor contributing to this rediscovery is that the majority of laboratories use one ionization source─electrospray ionization (ESI)─to conduct metabolomics studies. Although ESI is an efficient, widely adopted ionization method, its widespread use may contribute to the reidentification of known metabolites. Here, we present the use of a dielectric barrier discharge ionization (DBDI) for microbial metabolomics applications through the use of soft ionization chemical reaction in-transfer (SICRIT). Additionally, we compared SICRIT to ESI using two different Vibrio species: Vibrio fischeri, a symbiotic marine bacterium, and Vibrio cholerae, a pathogenic bacterium. Overall, we found that the SICRIT source ionizes a different set of metabolites than ESI, and it has the ability to ionize lipids more efficiently than ESI in the positive mode. This work highlights the value of using more than one ionization source for the detection of metabolites.

Major Ion Chemistry of Surface Water and Its Controlling Factors in Ebinur Lake Basin

The sustainable development of arid regions is significantly constrained by the availability of water resources, which play a crucial role in this context. It is necessary to deeply investigate and analyze the hydrochemical characteristics and major ion sources. This study, which was based on data from 183 water samples collected from the Jinghe River Basin, provided a comprehensive analysis of the river water hydrochemistry. The results show that the average TDSs (total dissolved solids) was measured at 49.8 mg·L−1. HCO3− (82.4%) and Ca2+ (77.1%) were the ions present in the highest abundances. The river water was classified as the HCO3−-Ca2+ hydrochemical type. The Gibbs diagrams indicated that the ion composition was primarily influenced by rock weathering. Additionally, the Na-normalized molar ratio diagrams suggested that the chemical composition was primarily governed by the weathering and dissolution of silicate rocks, while the carbonate rock dissolution played a lesser role. This study demonstrates a critical aspect of water resources quality evaluation, which is of great significance for the sustainable development, utilization and environmental protection of regional water resources.

Development of an Ultrasonic Nebulization System for an Inverse Low Temperature Plasma Ionization Source.

An effective nebulization and evaporation of a liquid sample, like in liquid chromatography, mass spectrometry (LC-MS) couplings, is an essential requirement for the ionization of analyte molecules in the gas phase by, for example, atmospheric pressure chemical ionization (APCI) or the novel low temperature plasma (LTP)-based ion source. These LTP-based ion sources have recently gained interest in the field of atmospheric pressure ion sources, as they can cover a wide range of polarity and molecular mass. They can be used in combination with separation techniques like liquid chromatography or used as an ambient ion source. However, commercial nebulizer systems are of course not constructed to fit to home-built LTP-based ion sources, and this was one incentive to develop a new nebulization system. Instead of an atmospheric pressure chemical ionization (APCI) nebulizer, two commercial nebulizers were disassembled and remodeled to be used as nebulizing systems in an LC-MS setup using an LTP-based ion source. Based on these results, a novel nebulizer system was subsequently developed. To further improve the degree of ionization, cones to focus the LC eluent spray on the plasma region, heating applications, and auxiliary nitrogen gas for dispersion of the solvent droplets were implemented. The LOD that could be calculated via the rule of three resulted in an average of 2.0 μg/L for the APCI-nebulizer and 41 μg/L for the USN. Both could be reduced to 1.4 and 18 μg/L, respectively, by using a TPI-configuration instead of an iLTP. The linearity was equally good for both types of nebulization devices. The final nebulizer could also be operated with a high water content and flow rates higher than those of the two previous ones, indicating an important improvement step.

Service spacecraft for space debris removal

The problem of space debris removal from the near-Earth space is being studied in almost every country taking part in space exploration. This is due to the global threat of critical increase in the number of space debris objects predicted for the near future, in particular as a result of significant growth in demand for multi-satellite constellations for various purposes. To date, researchers have proposed a large number of different methods for space debris removal. The work presented is the development of one of the promising contactless methods of space debris removal by an ion beam. The results of modeling and optimization of physical processes in the ion source to be mounted on board a service spacecraft that is necessary for implementing the considered method of space debris removal are presented. Besides, the results of thermal modeling and thermal mapping of the ion source during its operation are presented also, and the calculation results of its output parameters are compared to experimental data, which verified the small divergence angles of the generated ion beam. To assess the prospects of using a system for contactless space debris transportation by an ion beam using the obtained data on the operating parameters of the ion source, the trajectory design and mission analysis were carried out, which revealed the feasibility of removing seven space debris objects out of the protected region in geostationary orbit by a single service spacecraft. Besides, the preliminary service spacecraft design is presented.

High-Precision Mass Measurements of Neutron Deficient Silver Isotopes Probe the Robustness of the N=50 Shell Closure.

High-precision mass measurements of exotic ^{95-97}Ag isotopes close to the N=Z line have been conducted with the JYFLTRAP double Penning trap mass spectrometer, with the silver ions produced using the recently commissioned inductively heated hot cavity catcher laser ion source at the Ion Guide Isotope Separator On-Line facility. The atomic mass of ^{95}Ag was directly determined for the first time. In addition, the atomic masses of β-decaying 2^{+} and 8^{+} states in ^{96}Ag have been identified and measured for the first time, and the precision of the ^{97}Ag mass has been improved. The newly measured masses, with a precision of ≈1 keV/c^{2}, have been used to investigate the N=50 neutron shell closure, confirming it to be robust. Empirical shell-gap and pairing energies determined with the new ground-state mass data are compared with the state-of-the-art abinitio calculations with various chiral effective field theory Hamiltonians. The precise determination of the excitation energy of the ^{96m}Ag isomer in particular serves as a benchmark for abinitio predictions of nuclear properties beyond the ground state, specifically for odd-odd nuclei situated in proximity to the proton dripline below ^{100}Sn. In addition, density functional theory calculations and configuration-interaction shell-model calculations are compared with the experimental results. All theoretical approaches face challenges to reproduce the trend of nuclear ground-state properties in the silver isotopic chain across the N=50 neutron shell and toward the proton dripline.

High-performance liquid chromatography-tandem mass spectrometry was used to measure 20 antidepressants in human serum.

Aim: This study used high performance liquid chromatography-tandem mass spectrometry to quantify the blood concentrations of 20 antidepressants, such as bupropion and fluoxetine, in human serum samples.Methods: After direct precipitation with a 1:9 protein precipitant of methanol and acetonitrile, serum samples were examined using high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS). The material was separated using a Poroshell 120 EC-C18 column (3.0mm×50mm, 2.7μm) and gradient elution. The mobile phases were phase A 0.01% formic acid aqueous solution (containing 2mmol/ml ammonium acetate) and phase B methanol solution. A 0.45ml/min flow rate was used to divide the sample and inject 5μl. Electrospray ionization source positive ion mode and multiple reaction monitoring modes were used for analysis. Measurement was quantified using an internal standard technique.Results: Accuracy ranged from 90.3 to 114.3%, intra-day precision from 100.1 to 112.3%, inter-day precision from 100.4 to 112.6%, extraction recoveries from 85.5 to 114.5% and matrix effect from 85.6 to 98.7%.Conclusion: This approach is fast, accurate, sensitive and repeatable. It can identify 20 antidepressants in blood simultaneously. This can be used to monitor blood drug levels and medication metabolism.

Simultaneous multianalyte trace-level quantification of eight genotoxic nitrosamine impurities in valsartan Active Pharmaceutical Ingredient and tablet formulation using UFLC-MS/MS and greenness assessment

Valsartan, a widely prescribed antihypertensive drug, was identified for the presence of carcinogenic nitrosamine impurities in 2018, leading to product recalls worldwide and necessitating sensitive liquid and gas chromatographic methods for trace level detection of nitrosamine impurities. This study developed and validated an ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) method for the quantification of eight genotoxic nitrosamines (NDMA, NDEA, NDPA, NEIPA, NDIPA, NMBA, NDBA, and NMPA) in valsartan drug substance and tablet formulations. The method employed a triple quadrupole analyzer, atmospheric pressure chemical ionization (APCI) ionization source and multiple reaction monitoring (MRM) scan mode for the analysis. Chromatographic separation was achieved on a Phenomenex biphenyl column (150 × 4.6 mm, 3 µm) maintained at 55 °C. The mobile phase consisted of a binary gradient of solvent A (0.1 % formic acid in water) and solvent B (0.1 % formic acid in methanol), with a total run time of 20 min for the sensitive and specific detection of the analytes. Method validation demonstrated excellent linearity, recovery, precision, and sensitivity. The greenness of the developed analytical method was critically assessed through comprehensive evaluations using the GAPI, AGREE, and AES metrics and the results obtained are compared with the reported methods in the literature. This novel UFLC-MS/MS method offers a reliable and sensitive approach for routine quality control analysis of nitrosamine impurities in Valsartan drug substance and tablet formulations.

Comparative Pharmacokinetics and Tissue Distribution of Hexahydrocurcumin Following Intraperitoneal vs Oral Administration in Mice Using LC-MS/MS.

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to determine hexahydrocurcumin (HHC) levels in mouse plasma, brain, liver, and kidneys using a negative ion mode electrospray ionization (ESI) source. Demonstrating a lower limit of quantification (LLOQ) of 5 ng/mL, the method showed excellent linearity across a concentration range of 5-500 ng/mL in all tested matrices. Precision evaluations reported a coefficient of variation (CV%) of less than 13.19% for both intraday and interday measurements, while accuracy ranged from 95.13 to 105.07% across all quality control levels. HHC extraction recovery was consistently observed between 70.18 and 93.28%, with a CV% deviation of less than 15%. In the pharmacokinetic evaluation of HHC in mice following a single intraperitoneal (IP) or oral administration, a noncompartment analysis was utilized. After IP administration (40 mg/kg), the C max value was 47.90 times higher than that achieved via oral administration. Peak plasma concentrations were observed approximately 5 min post-IP and 15 min post-oral dosing. The observed half-lives after these administrations were approximately 1.52 and 2.17 h for IP and oral routes, respectively. Oral administration revealed a relative bioavailability of only 12.28% compared with the IP route. Furthermore, following IP administration, the half-life values in brain, liver, and kidney were not significantly different but more than the half-life value found in plasma. The liver and kidney exhibited the highest concentrations of HHC, while the brain showed the least, suggesting that the hydrophobic nature of HHC impedes its passage through the blood-brain barrier. This study is the first to provide detailed insights into the pharmacokinetics and tissue distribution characteristics of HHC following oral and IP administration in mice, setting the stage for further focus on HHC as a potential new drug candidate.