Optimisation of whole blood and plasma manganese assay by ICP-MS without use of a collision cell

Author(s):  
Claire Richardson ◽  
Edward Roberts ◽  
Simon Nelms ◽  
Norman B. Roberts

AbstractManganese (Mn) toxicity has been reported in patients receiving total parenteral nutrition. To avoid unnecessary exposure it is recommended by NICE (National Institute for Clinical Excellence) that blood Mn concentrations are monitored. The aim of the study was to develop a method using inductively coupled plasma mass spectrometry (ICP-MS) for the reliable determination of Mn in plasma and whole blood, as indices of acute and chronic exposure.Whole blood and plasma samples were prepared by appropriate dilution (diluent containing 0.005% Triton X-100, 0.2% propan-2-ol, 0.2% butan-1-ol and 1% nitric acid) addition of an internal standard gallium, followed by centrifugation to remove cell debris. Thermo Fisher Scientific ExCell and X Series ICP-MS instruments were used to define and correct for polyatomic interference on Mn assay.Mn was quantified at mass 55 using aqueous calibration and the polyatomic interference from FeH was successfully eliminated by modified (Xt) skimmer cones but not with the collision cell (collision gas 7% HA method has been developed using ICP-MS for the analysis of whole blood and plasma Mn incorporating a novel method of eliminating interference by utilizing the different geometries of the Xt interface cones. The procedure is simple and robust with good precision and recovery over a wide dynamic range.

2001 ◽  
Vol 8 (4) ◽  
pp. 776-784 ◽  
Author(s):  
Christophe Camilla ◽  
Laurent Mély ◽  
Antoine Magnan ◽  
Brice Casano ◽  
Sabine Prato ◽  
...  

ABSTRACT The ability of flow cytometry to resolve multiple parameters was used in a microsphere-based flow cytometric assay for the simultaneous determination of several cytokines in a sample. The flow cytometer microsphere-based assay (FMBA) for cytokines consists of reagents and dedicated software, specifically designed for the quantitative determination of cytokines. We have made several improvements in the multiplex assay: (i) dedicated software specific for the quantitative multiplex assay that processes data automatically, (ii) a stored master calibration curve with a two-point recalibration to adjust the stored curve periodically, and (iii) an internal standard to normalize the detection step in each sample. Overall analytical performance, including sensitivity, reproducibility, and dynamic range, was investigated for interleukin-4 (IL-4), IL-6, IL-10, IL-12, gamma interferon (IFN-γ), and tumor necrosis factor alpha. These assays were found to be reproducible and accurate, with a sensitivity in the picograms-per-milliliter range. Results obtained with FMBA correlate well with commercial enzyme-linked immunosorbent assay data (r > 0.98) for all cytokines assayed. This multiplex assay was applied to the determination of cytokine profiles in whole blood from atopic and nonatopic patients. Our results show that atopic subjects' blood produces more IL-4 (P = 0.003) and less IFN-γ (P = 0.04) than the blood of nonatopic subjects. However, atopic asthmatic subjects' blood produces significantly more IFN-γ than that of atopic nonasthmatic subjects (P = 0.03). The results obtained indicate that the FMBA technology constitutes a powerful system for the quantitative, simultaneous determination of secreted cytokines in immune diseases.


2019 ◽  
Vol 89 (6) ◽  
pp. 965
Author(s):  
Т.К. Нурубейли ◽  
К.З. Нуриев ◽  
З.К. Нурубейли ◽  
K.Б. Гурбанов

In work on the example of a number of elements in whole blood and urine with use of ICP-MS with the quadruple Agilent-7700 analyzer the attempt of elimination of influence of not spectralm atrix effect leading to suppressiono f intensity of an analytical signal at the device exit is made. It is shown that the main role in emergence of not spectral matrix effect is played both acids also by composition of salt in solution, and the organic matters which are a part of the exemplar. Influence of acid, salt and organic structure of a matrix of whole blood and urine on understating of results of definition of a number of elements is estimated. It is shown also that the internal standard (IS) has to be chosen proceeding from proximity of the first potential of ionization of VS and a defined element. Deposits of not spectral matrix effects in distortion of results of the analysis of biological liquids are investigated and estimated and it is established that, dependenceo f matrix effect of saltsa nd aciditieso f a matrix, and also on a duty of the device has the additive character


2019 ◽  
Author(s):  
Ingo Strenge ◽  
Carsten Engelhard

<p>The article demonstrates the importance of using a suitable approach to compensate for dead time relate count losses (a certain measurement artefact) whenever short, but potentially strong transient signals are to be analysed using inductively coupled plasma mass spectrometry (ICP-MS). Findings strongly support the theory that inadequate time resolution, and therefore insufficient compensation for these count losses, is one of the main reasons for size underestimation observed when analysing inorganic nanoparticles using ICP-MS, a topic still controversially discussed.</p>


2020 ◽  
Vol 17 ◽  
Author(s):  
LiJuan Wang ◽  
Yan Liu ◽  
Rui Li ◽  
DongXian He

Objectives: Triptolide (TPL) has been shown to have a good clinical effect on rheumatoid arthritis (RA). We designed TPL microspheres (TPL-MS) and investigated its metabolic behavior in human, dog, rabbit and rat liver microsomes (HLM, DLM, RLM and SDRLM) with UPLC-MS/MS method. Methods: First, a UPLC-MS/MS method was established to measure concentration of TPL in samples. The sample was separated on a C18 column (2.1×100 mm, 1.8μm) and eluted with a gradient elution. The precursor ion/product ion were m/z 378.1/361.0 for TPL and 260.0/116.2 for the internal standard. Then T1/2, Vmax and CLint were calculated from the above data. Finally, the metabolites of TPL-MS were identified by high-resolution UPLC-MS/MS. The sample was separated on a C18 column (2.1×100 mm, 2.2 μm) and eluted with isocratic elution. Mass spectrometric detection was carried out on a thermo Q-exactive mass spectrometer with HESI. The scanning range of precursor ions was from m/z 50 to m/z 750. Result and Discussion: Through several indicators including standard curve, precision, accuracy, stability, matrix effect and recovery rate, the enzymatic kinetics parameters including T1/2, Vmax and CLint were completed. Several metabolites of TPL-MS were identified. Conclusion: UPLC-MS/MS method is an accurate and sensitive method for determination of TPL in liver microsome samples with good precision, accuracy and stability. The variation of parameters indicated that the microspheres can delay the elimination of TPL in liver microsomes. The metabolism of TPL-MS varied among species, but no new metabolites appeared.


Molecules ◽  
2021 ◽  
Vol 26 (2) ◽  
pp. 479
Author(s):  
Shihan Wang ◽  
Yuanshuai Gan ◽  
Hong Kan ◽  
Xinxin Mao ◽  
Yongsheng Wang

As one of the featured products in northeast China, Oviductus Ranae has been widely used as a nutritious food, which contains a variety of bioactive unsaturated fatty acids (UFAs). It is necessary to establish a scientific and reliable determination method of UFA contents in Oviductus Ranae. In this work, six principal UFAs in Oviductus Ranae, namely eicosapentaenoic acid (EPA), linolenic acid (ALA), docosahexaenoic acid (DHA), arachidonic acid (ARA), linoleic acid (LA) and oleic acid (OA), were identified using UPLC-MS/MS. The UFAs identified in Oviductus Ranae were further separated based on the optimized RP-HPLC conditions. Quantitative analysis of multi-components by single-marker (QAMS) method was implemented in content determination of EPA, ALA, DHA, ARA and OA, where LA was used as the internal standard. The experiments based on Taguchi design verified the robustness of the QAMS method on different HPLC instruments and chromatographic columns. The QAMS and external standard method (ESM) were used to calculate the UFA content of 15 batches of Oviductus Ranae samples from different regions. The relative error (r < 0.73%) and cosine coefficient showed that the two methods obtained similar contents, and the method validations met the requirements. The results showed that QAMS can comprehensively and effectively control the quality of UFAs in Oviductus Ranae which provides new ideas and solutions for studying the active components in Oviductus Ranae.


2017 ◽  
Vol 43 ◽  
pp. 38-45 ◽  
Author(s):  
Brice Yedomon ◽  
Alain Menudier ◽  
Florence Lecavelier Des Etangs ◽  
Ludovic Anani ◽  
Benjamin Fayomi ◽  
...  
Keyword(s):  

Author(s):  
Michael Fitzpatrick ◽  
Paul Bonnitcha ◽  
Van Long Nguyen

Abstract Objectives In the clinical setting, the analysis and quantification of vitamin C (ascorbic acid) poses several challenges including analyte instability and poor retention by reverse phase HPLC systems. In this article we describe a rapid hydrophilic interaction chromatography ultraviolet method for the measurement of total vitamin C in plasma which overcomes these issues. Methods Ascorbic acid and the internal standard were separated under isocratic conditions using a Waters BEH-Amide column and a mobile phase containing 0.005 M potassium phosphate in 80% acetonitrile. Results The proposed method was validated and showed good precision (coefficient of variation <5%), accuracy (>99%), and analyte stability after extraction (>24 h). Conclusions The simple sample preparation allows full automation and rapid analytical run times of the assay and is therefore suitable for a high-throughput clinical chromatography laboratory.


2017 ◽  
Vol 10 (5) ◽  
pp. 1823-1830 ◽  
Author(s):  
Marin S. Robinson ◽  
Irena Grgić ◽  
Vid S. Šelih ◽  
Martin Šala ◽  
Marsha Bitsui ◽  
...  

Abstract. A widely used instrument for collecting size-segregated particles is the micro-orifice uniform deposit impactor (MOUDI). In this work, a 10-stage MOUDI (cut-point diameter of 10 µm to 56 nm) was used to collect samples in Ljubljana, Slovenia, and Martinska, Croatia. Filters, collected with and without rotation, were cut in half and analyzed for nine elements (As, Cu, Fe, Ni, Mn, Pb, Sb, V, Zn) using laser ablation ICP-MS. Elemental image maps (created with ImageJ) were converted to concentrations using NIST SRM 2783. Statistical analysis of the elemental maps indicated that for submicron particles (stages 6–10), ablating 10 % of the filter (0.5 cm2, 20 min ablation time) was sufficient to give values in good agreement (±10 %) to analysis of larger parts of the filter and with good precision (RSE < 1 %). Excellent sensitivity was also observed (e.g., 20 ± 0.2 pg m−3 V). The novel use of LA-ICP-MS, together with image mapping, provided a fast and sensitive method for elemental analysis of size-segregated MOUDI filters, particularly for submicron particles.


2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Andréia Ávila Soares de Oliveira ◽  
Marilesia Ferreira de Souza ◽  
André van Helvoort Lengert ◽  
Marcelo Tempesta de Oliveira ◽  
Rossana Batista de Oliveira Godoy Camargo ◽  
...  

This study aims to evaluate the effects of polymorphisms in glutathione (GSH-) related genes (GSTM1,GSTT1,GSTP1,GCLM, andGCLC) in the distribution of Hg in the blood compartments in humans exposed to methylmercury (MeHg). Subjects (n=88), exposed to MeHg from fish consumption, were enrolled in the study. Hg species in the plasma compartment were determined by LC-ICP-MS, whereas genotyping was performed by PCR assays. Mean total Hg levels in plasma (THgP) and whole blood (THgB) were10±4.2and37±21, whereas mean evels of plasmatic MeHg (MeHgP), inorganic Hg (IHgP), and HgP/HgB were4.3±2.9,5.8±2.3 µg/L, and0.33±0.15, respectively.GSTM1andGCLCpolymorphisms influence THgP and MeHgP (multivariate analyses,P<0.050). Null homozygotes forGSTM1showed higher THgP and MeHgP levels compared to subjects withGSTM1(THgPβ=0.22,P=0.035; MeHgPβ=0.30,P=0.050) and persons carrying at least one T allele forGCLChad significant higher MeHgP (β=0.59,P=0.046). Also, polymorphicGCLMsubjects had lower THgP/THgB than those with the nonvariant genotype. Taken together, data of this study suggest that GSH-related polymorphisms may change the metabolism of MeHg by modifying the distribution of mercury species iin plasma compartment and the HgP/HgB partitioning.


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