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PubMed2000

Correction of species transformations in the analysis of Cr(VI) in solid environmental samples using speciated isotope dilution mass spectrometry

Speciation of Cr(VI) in solid environmental samples is challenging because of the transformations between Cr(VI) and Cr(III). EPA method 3060A completely extracts Cr(VI) in a hot alkaline solution and preserves the solublized Cr(VI). This procedure, however, can oxidize Cr(III) in some chemical forms. On the other hand, the reverse transformation may occur during neutralization and acidification following the extraction step. We developed a method that is capable of monitoring and correcting for such bidirectional species transformations to determine Cr(VI) in solid samples. In this method, we spike a sample with a 53Cr(VI) spike (enriched in 53Cr) and a isoCr(III) spike (enriched in 50Cr). The large quantity of isoCr(III) in an easily oxidizable form competes with sample Cr(III) in the oxidization, reducing the method-induced oxidation of sample Cr(III). This method also corrects for the reduction of Cr(VI). The theory is presented and is evaluated experimentally. The analysis of chromite ore processing residue, fly ash, and standard reference material SRM 1645 showed that the oxidation of sample Cr(III) could cause positive biases as high as 163% if no correction is performed.

Journal Article↗
PubMed2001

Comparison of three coupled gas chromatographic detectors (MS, MIP-AES, ICP-TOFMS) for organolead speciation analysis.

An automatic unit for the screening of rainwater is used for the determination of organolead compounds using different detectors coupled to a gas chromatograph. A systematic overview is given of the advantages and disadvantages of several detectors (electron ionization mass spectrometry, EI-MS; microwave induced plasma atomic emission spectrometry, MIP-AES; and inductively coupled plasma time-of-flight mass spectrometry, ICP-TOFMS, for the speciation of organolead compounds on the basis of sensitivity, selectivity and reliability. C60 fullerene and RP-C18 were used as sorbent materials for these compounds. The primary assets of the fullerene sorbent, as compared to C18 sorbent, are high sensitivity and selectivity resulting from efficient adsorption due to large surface area and interstitial volume. Among the detection systems, GC/ ICP-TOFMS is the most sensitive, with absolute detection limits of approximately 15 fg of organolead compounds (as lead) using 5-mL sample volumes. Except for diethyllead, similar sensitivities were obtained by MIP-AES. GC/MS is intrinsically the most specific option, because the species are detected directly from molecular information. The precision is similar for all detectors. The screening of rainwater from different locations showed that samples collected in countries in which leaded gasolines are now banned contain organolead species at concentrations below 2 pg/ mL, levels that can be detected only for sample volumes of 25 mL and using MIP-AES or ICP-TOFMS as detectors, their determination being impossible by GC/MS.

Journal Article↗
PubMed2001

Speciation and identification of organoselenium metabolites in human urine using inductively coupled plasma mass spectrometry and tandem mass spectrometry.

A method for speciation and identification of organoselenium metabolites found in human urine samples using high performance liquid chromatography/inductively coupled plasma mass spectrometry (HPLC/ICP-MS) and tandem mass spectrometry (MS/MS) is described. Reversed-phase chromatographic separation was used for sample fractionation with the ICP-MS functioning as an element-selective detector, and six distinct selenium-containing species were detected in a human urine sample. Fractions were then collected and analyzed using a triple quadrupole mass spectrometer with electrospray ionization and collision-induced dissociation to obtain structural information. The first two fractions were identified specifically as selenomethionine and selenocystamine, estimated to be present at approximately 11 and 40 ppb, respectively. To the best of our knowledge, this is the first time these two metabolites have been positively identified in human urine.

Chromatography, High Pressure Liquid↗
PubMed2001

A method for the quantitative analysis of iron speciation in meat by using a combination of spectrophotometric methods and high-performance liquid chromatography coupled to sector field inductively coupled plasma mass spectrometry.

The determination of the heme and non-heme iron fractions in raw and cooked beef steak by using spectrophotometric methods and high-performance liquid chromatography coupled to a double-focusing sector field inductively coupled plasma mass spectrometer (HPLC-SF-ICPMS) is reported. Size exclusion chromatography coupled to SF-ICPMS was used to measure the iron-containing biomolecules in the samples. This approach allowed for the direct on-line detection of the most abundant iron isotope 56Fe without interference from 40Ar16O. The HPLC-ICPMS results for the iron speciation analysis of a raw beef steak, used as an analytical quality control (AQC) sample, showed that the main iron biomolecule present was the heme iron-containing protein myoglobin. For the AQC sample, the agreement among the HPLC-ICPMS method, the non-heme iron spectrophotometric method, and the total iron concentration showed 100% recovery of iron. The sum of the different iron-containing compounds determined using the developed HPLC-ICPMS method accounted for all the iron-containing compounds extracted. The analysis of myoglobin in steak by HPLC-ICPMS showed that on cooking the concentration was reduced by 85%. However, a spectrophotometric method specific for heme iron showed that it was still intact, even after heating to 80 degrees C. The measurement of the total iron in the cooked steak and the HPLC extracts by inductively coupled plasma optical emission spectroscopy (ICP-OES) indicated that the extraction method for the HPLC analysis was no longer applicable and that loss of the heme group from the protein rendered it incompatible with the size exclusion separation. The detection limit (concentration equivalent to 3 times the baseline for a blank injection) of the HPLC-ICPMS method was 2.4 ng as iron. The results demonstrate that a combination of analytical methods can be used to provide valuable information about dietary levels of nutritionally important metal-containing compounds as well as the efficiency of established extraction methods for raw and cooked meat samples.

Animals↗
PubMed2001

Speciation of aluminum in rainwater using a fluoride ion-selective electrode and ion-exchange chromatography with fluorometric detection of the aluminum-lumogallion complex.

Soluble aluminum in rainwater was separated into three categories: free aluminum (Al3+), fluoride complexes (sum of AlF2+ and AlF2+), and other forms of aluminum. The free form of the aluminum ion (Al3+) was directly obtained from the separation data of aluminum species according to their charge using gradient elution cation-exchange chromatography. The aluminum fluoride complexes were estimated by combining the data of the free and total fluoride determined using a fluoride ion-selective electrode, with the assumption that 2+ charged aluminum species consisted only of AlF2+. The rest of the aluminum species had a 1+, neutral, or negative charge and mainly consisted of organic complexes. The origin of the organically bound aluminum is discussed. The concentration range of the total dissolved fluoride and aluminum in the rainwater samples was usually in the micromolar to submicromolar range, and the ratio of [T-F]/[T-Al] was found to be between 1 and 4. The speciation of dissolved aluminum into three categories was carried out on the basis of data of 15 rainwater samples collected in the city of Otsu.

Acid Rain↗
PubMed2002

Initial studies of selenium speciation in Brassica juncea by LC with ICPMS and ES-MS detection: an approach for phytoremediation studies.

Various Brassica species accumulate Se into the thousands of ppm. This suggests some of them as candidates for Se phytoremediation. Brassica juncea (Indian mustard) was used to accumulate selenium by growing with sodium selenite as the selenium source under hydroponic conditions resulting in Se accumulation of up to hundreds of ppm in various parts of the plant. To date, few selenium speciation studies have been done in plants, with most studies reporting total selenium concentration in various parts of the plant. Se species extraction was evaluated by several digestion/extraction procedures, including the use of HCl, Tris-HCl buffer, and enzymatic hydrolysis (using proteinase K and protease XIV). The best extraction was obtained with proteinase K (extracting approximately 75% of the total Se present in the plant). Some of the species produced by the plant, such as selenomethionine, can be identified at ppb levels by RP-HPLC-ICPMS, since standards are readily available. Others needed to be further characterized by ES-MS. Enzymatic hydrolysis releases mostly Se-methionine from juncea leaves, although other Se-containing species can also be observed by HPLC-ICPMS. In this initial study, the possible identification (by ES-MS) of a small chromatographic peak containing a Se-S bridged seleno amino acid with a structure similar to cystine is suggested.

Brassica↗
PubMed2003

Speciation of dimethylarsinous acid and trimethylarsine oxide in urine from rats fed with dimethylarsinic acid and dimercaptopropane sulfonate.

Speciation of arsenic in urine from rats treated with dimethylarsinic acid (DMA(V)) alone or in combination with dimercaptopropane sulfonate (DMPS) were studied. Methods were developed for the determination of the methylarsenic metabolites, especially trace levels of dimethylarsinous acid (DMA(III)) and trimethylarsine oxide (TMAO), in the presence of a large excess of DMA(V). Success was achieved by using improved ion-exchange chromatographic separation combined with hydride generation atomic fluorescence detection. Micromolar concentrations of DMA(III) were detected in urine of rats fed with a diet supplemented with either 100 microg/g of DMA(V) or a mixture of 100 microg/g of DMA(V) and 5600 microg/g of DMPS. No significant difference in the DMA(III) concentration was observed between the two groups; however, there was a significant difference in TMAO concentrations. Urine from rats fed with the diet supplemented with DMA(V) alone contained 73 +/- 30 microM TMAO, whereas urine from rats fed with the diet supplemented with both DMA(V) and DMPS contained only 2.8 +/- 1.4 microM TMAO. Solutions containing mixtures of 100 microg/L DMA(V) or TMAO and 5600 microg/L DMPS did not show reduction of DMA(V) and TMAO. The significant decrease (p < 0.001) of the TMAO concentration in rats administered with both DMA(V) and DMPS suggests that DMPS inhibits the biomethylation of arsenic.

Administration, Oral↗
PubMed2005

Effect of model ligands on iron redox speciation in natural waters using flow injection with luminol chemiluminescence detection.

The effects of dissolved organic compounds on the determination of nanomolar concentrations of Fe(II) have been compared using two luminol-based flow injection chemiluminescence (FI-CL) methods. One used the direct injection of sample into the luminol reagent stream, and the other incorporated on-line solid-phase extraction of the analyte on an 8-hydroxyquinoline microcolumn. The CL signals from analyses of dissolved iron species (Fe(II) and Fe(III)) with model ligands and organic compounds were examined in high-purity water and seawater. The organic compounds included natural reducing agents (e.g., ascorbic acid), nitrogen sigma-donor/pi-acceptor compounds (e.g., 1,4-dipyridine, protoporphyrin IX), aromatic compounds (e.g., 1,4-dihydroxybenzene), synthetic iron chelators (e.g., EDTA), and natural iron binding compounds (e.g., desferrioxamine B, ferrichrome A). Fe(II) determinations for both luminol FI-CL methods were affected by submicromolar concentrations of redox-active compounds, strong iron binding ligands (i.e., log K(FeL) > 6), and compounds with electron-donating functional groups in both high-purity water and seawater. This was due to reactions between organic molecules and iron species before and during analysis, rather than chemiluminescence caused by the individual organic compounds. In addition, the effects of strong ligands and size speciation on Fe(II) recoveries from seawater following acidification (pH 2) and reduction (100 microM sodium sulfite) were investigated.

Journal Article↗
PubMed2005

Speciation of chromium(III) and cobalt(III) (amino)carboxylate complexes using capillary electrophoresis.

Capillary electrophoresis (CE) can very efficiently resolve different dissolved metal ion species as long as rates of ligand exchange are slow relative to time scales required for electromigration. Here, we detail the separation of several Cr(III) and Co(III) complexes with the multidentate chelating agents iminodiacetic acid, nitrilotriacetic acid, trans-1,2-cyclohexanediaminetetracetic acid, N-(2-hydroxyethyl)ethylenediaminetriacetic acid, trimethylenediaminetetraacetic acid, and ethylenediaminetetraacetic acid. Successes in speciating some Ni(II) and Co(II) complexes are also reported. For Cr(III) and Co(III), subtle differences in metal ion-chelating agent stereochemistry, chelating agent denticity, and number of bridging ligands are discernible due to the high resolving power of CE. New peaks and heightened baselines were encountered when a pH buffer with strong complexing properties (orthophosphate) was employed in the background electrolyte. For this reason, we recommend using pH buffers with very weak or negligible complex properties (e.g., MES and MOPS).

Journal Article↗
PubMed2004

Hydride generation interface for speciation analysis coupling capillary electrophoresis to inductively coupled plasma mass spectrometry.

A novel hydride generation (HG) interface for coupling capillary electrophoresis (CE) with inductively coupled plasma mass spectrometry (ICPMS) is presented in this work. The CE-HG-ICPMS interface was applied to the separation and quantitation of common arsenic species. Lack of a commercially available HG interface for CE-ICPMS led to a three concentric tube design allowing alleviation of back pressure commonly observed in CE-HG-ICPMS. Due to the high sensitivity and element-specific detection of ICPMS, quantitative analysis of As(III), As(V), monomethylarsonic acid, and dimethylarsinic acid was achieved. Optimization of CE separation conditions resulted in the use of 20 mmol L(-1) sodium borate with 2% osmotic flow modifier (pH 9.0) and -20 kV applied potential for baseline resolution of each arsenic species in the shortest time. Hydride generation conditions were optimized through multiple electrophoretic separation analyses with 5% HCl and 3% NaBH(4) (in 0.2% NaOH) determined to be the optimum conditions. After completion of system optimization, detection limits obtained for the arsenic species were less than 40 ng L(-1) with electromigration time precision less than 1% within a total analysis time of 9.0 min. Finally, the interface was used for speciation analysis of arsenic in river and tap water samples.

Arsenic↗
PubMed2005

Speciation-capable field instrument for the measurement of arsenite and arsenate in water.

Hydride generation to form arsine and in-line preconcentration of the arsine into an alkaline KMnO4 receiver followed by molybdenum blue (MB) colorimetric determination of the arsenate formed is proposed for the highly sensitive and separate measurement of total inorganic As and As(III). Reduction of As to AsH3 is carried out by NaBH4; when the reduction is carried out at pH 1, all the inorganic As is reduced to AsH3, and when carried out at pH 7, only As(III) is reduced. Reductions at the two different pH levels are carried out in two different arsine generators simultaneously using constant addition of NaBH4 with solenoid pumps. The AsH3 is collected by individual porous membrane diffusion scrubbers filled with a stationary solution of KMnO4, and the contents of the two scrubbers sequentially enter a flow analysis stream. MB is formed by merging with a ammonium molybdate-ascorbic acid reagent, passing through a heated reactor, and is then measured by a LED/photodiode-based absorbance detector. Robustness was confirmed for total As using three types of certified natural water samples. Speciation analysis data from well water samples analyzed by this method agree well with HPLC-ICPMS measurements in a different laboratory. The system has been successfully applied to field measurements of As(III) and As(V), where levels were significantly below 1 mug/L. For a 20-mL sample, the limits of detection (LODs) for this inexpensive instrument are 0.3 microg/L for both As(III) and total As. When an 80-mL sample is analyzed, LODs are 0.07 microg/L As(III) and 0.09 microg/L total As. The general approach should be applicable to many other analyte species of interest that can be isolated from the matrix by the formation of a suitable volatile compound that can be recaptured.

Journal Article↗
PubMed2005

Speciation of organometallic compounds in environmental samples by gas chromatography after flow preconcentration on fullerenes and nanotubes.

The development of a simple speciation method for the determination of lead (trimethyllead(I), dimethyllead(II), triethyllead(I), and diethyllead(II)), mercury (methylmercury(I), ethylmercury(I), mercury(II)), and tin (n-butyltin(III), di-n-butyltin(II), tri-n-butyltin(I), tin(IV)) compounds in environmental samples was described. The potential of C70 fullerenes and multiwalled carbon nanotubes (MWNTs) as sorbents was investigated for the first time; this study revealed that there are no significant differences between them in terms of sensitivity, selectivity, precision, and reusability. Comparative studies showed that MWNTs and C60 and C70 fullerenes were superior to graphitized carbon black and RP-C18 for the extraction of the 11 compounds studied. The accuracy of the MWNT method was evaluated from recovery values with two standard reference coastal sediments, and good concordance in the results were obtained. Detection limits of 0.5-2 pg/mL were obtained when using a sorbent column containing 160 mg of MWNTs (sample breakthrough, 50 mL of water). The method was successfully applied to the determination of lead, mercury, and tin compounds in water and coastal sediment samples with satisfactory results.

Chromatography, Gas↗
PubMed2006

Chemical speciation of iron in seawater by cathodic stripping voltammetry with dihydroxynaphthalene.

The chemical speciation of iron in seawater is determined by cathodic stripping voltammetry using 2,3-dihydroxynaphthalene (DHN) as adsorptive and competing ligand. The optimized conditions include a DHN concentration of 0.5-1 microM, seawater at its original pH of 8, and equilibration overnight. The alpha-coefficient for DHN (=[FeDHN]/[Fe']) was calibrated against EDTA giving values of 166 for 0.5 microM DHN and 366 at 1 microM DHN and a value of 8.51 +/- 0.07 for log K'(Fe'DHN). The dissociation of the natural iron species FeL was found to have a characteristic reaction time of 50 min, indicating that titrations should be equilibrated overnight rather than the shorter periods sometimes used onboard ship. The method was applied to samples from the Pacific giving ligand concentrations of 1.1 and 1.6 nM for deep and surface waters, respectively, with an average value for log K'(FeL) of 11.9 +/- 0.3 compared to a value of 11.5 for the siderophore deferoxamine. The results are similar to those obtained previously for similar samples, but the new method has much greater sensitivity for iron than previous methods, leading to lower limits of detection and shorter analysis time.

Journal Article↗
PubMed2006

A high-efficiency photooxidation reactor for speciation of organic arsenicals by liquid chromatography-hydride generation-ICPMS.

A novel postcolumn photooxidation reactor with remarkably high efficiency was developed. It was installed into a system of liquid chromatography (LC) combined with inductively coupled plasma mass spectrometry (ICPMS) using a hydride generation (HG) technique to enable sensitive speciation of organic arsenicals. An LC eluent was passed into a reaction tube that runs through a low-pressure mercury lamp of a high-efficiency photooxidation (HEPO) reactor. It provided efficient irradiation with vacuum ultraviolet light at 185 nm, which induced oxidative decomposition of persistent organic arsenicals, for example, arsenobetaine, to the final product, arsenate, for an extremely short time, 3.5 s, without using any oxidizing agents. That arsenate was subsequently detectable by HG-ICPMS. In contrast, conventional photooxidation reactors require more than 100 s for completion, even when using a peroxodisulfate solution as an oxidizing agent. Because of the absence of broadening and dilution of the LC-separated peaks caused by mixing with the oxidant solution, the detection limits for 10 arsenic species including the persistent organic arsenicals by the proposed LC-HEPO-HG-ICPMS ranged from 2.3 to 18 ng of As/L, which were about one-tenth as low as those by LC-ICPMS. The proposed method revealed for the first time the occurrence of 20 arsenic species, including the unknown trace species, which were undetectable by LC-ICPMS and LC-HG-ICPMS, in human urine.

Arsenicals↗
PubMed2006

In vivo investigation of the distribution and the local speciation of selenium in Allium cepa L. by means of microscopic X-ray absorption near-edge structure spectroscopy and confocal microscopic X-ray fluorescence analysis.

In this work, microscopic X-ray absorption near-edge structure spectroscopy (mu-XANES) and confocal microscopic X-ray fluorescence analysis (mu-XRF) were used for the in vivo determination of the distribution of total selenium and for the local speciation of selenium in roots and leaves of onion. Selected Allium cepa L. plants were grown hydroponically in a standard medium containing inorganic selenium compounds (selenite or selenate). The measurements were performed in vivo, that is, on living plants without the need for any form of sampling or sample pretreatment and without the necessity for cutting plant tissues into pieces. Distinct energy differences of the XANES spectra of various selenium reference compounds having different oxidation states allow adjusting the excitation energies used for mu-XRF mapping in such a manner that the distribution of selenium in various oxidation states is obtained with a spatial resolution of a few tens of micrometers within the virtual cross section of the onion tissues. We find that the ratio of inorganic to amino acid selenium compounds differs in various subparts of the plant. Detailed in vivo investigation of the distribution of various selenium species in virtual cross sections of root tips and green leaf shows that the selenium transport takes place via different mechanisms, depending on the nature of the selenium compounds originally taken up.

Amino Acids↗
PubMed2006

Elemental speciation by parallel elemental and molecular mass spectrometry and peak profile matching.

Trace elemental speciation in complex, real-world matrixes is a daunting task because of the low concentration of metals/metalloids and the correspondingly high molecular chemical noise. We constructed a liquid chromatography parallel elemental and molecular mass spectrometry (PEMMS) system and evaluated the use of peak elution profiles to identify trace molecular species containing specific heteroatoms, using the case of Se in yeast. We demonstrate that it is possible to use the HPLC-inductively coupled plasma (ICP)MS peak profile (retention time, width) to identify candidate ions with matching peak profiles in the molecular MS data. Proof of principle was demonstrated by C18 separation of three Se-amino acid standards (0.005-15 ppm as Se). The molecular MS (atmospheric pressure chemical ionization time-of-flight, APCI-TOF-MS) data set was converted into selected ion chromatograms of 0.05 Th width. ICPMS and APCI-TOF-MS ion chromatograms were fit by the Haarhoff-VanderLinde function using the following parameters: area, retention time, width, and skew. The ICPMS fit parameters were more reproducible than the APCI-TOF-MS fit parameters from run to run, and the APCI-TOF-MS signal was expected to limit correlation in most circumstances. Retention time and width were found to correlate well between the two MS systems for APCI-TOF-MS peaks with signal-to-fit-error (S/FE) of >25. Correction factors for differences in flow path length and peak broadening were required. The normalized correction factors were species and concentration independent and were stable from run to run. The skew parameter was found to be highly susceptible to noise and was not generally useful in matching ICPMS and APCI-TOF-MS peaks. An artificially noisy sample was generated by spiking 30 ppb Se-methionine (SeMet) and 5 ppb Se-methylselenocysteine (SeMSC) with unselenized yeast extract and run by PEMMS. The PEMMS software was able to detect four molecular MS peaks associated with SeMet and two for SeMSC, while filtering out >40 coeluting spectral peaks associated with chemical noise in each sample. In summary, we have demonstrated that correlated information in peak shape between parallel detectors can facilitate detection of trace elemental species in complex matrixes.

Journal Article↗
PubMed2006

Consequences of vapor enhancement on selenium speciation analysis by HPLC/ICPMS.

Recent work has shown the presence of volatile selenium metabolites in human urine and suggested that these compounds could compromise quantitative selenium analyses by ICPMS. We show that with a commonly used sample introduction system (pneumatic nebulizer and spray chamber), two volatile selenium species recently identified in urine, namely, dimethyl selenide and dimethyl diselenide, gave greatly increased ICPMS responses (up to 58-fold) relative to selenite, an effect related to their volatilization in the spray chamber resulting in enhanced transport to the plasma. The quantitative consequences of this effect were demonstrated by measurement of total selenium and selenium species in certified reference material, NIES CRM 18 human urine. Direct flow injection analysis of the urine gave a total selenium concentration more than 2-fold higher than the certified value. These data suggested that NIES CRM 18 may contain part of its selenium as volatile species, and subsequent reversed-phase HPLC/ICPMS showed the presence of dimethyl selenide in addition to selenosugars and trimethylselenonium ion. Although the practice of quantifying unidentified chromatographic peaks against those of known compounds is common in speciation analysis, this approach when applied to NIES CRM 18 gave a value for the sum of selenium species which was twice the certified total selenium concentration. This work shows that the presence of volatile selenium species in urine precludes the use of flow injection analysis for total selenium measurements and imposes severe restrictions on the quantification of urinary selenium metabolites. In addition, it raises broader issues of the validity of the "dilute and shoot" approach to the determination of metals in clinical analysis of biological fluids.

Chromatography, High Pressure Liquid↗
PubMed1998

Purge-and-trap isothermal multicapillary gas chromatographic sample introduction accessory for speciation of mercury by microwave-induced plasma atomic emission spectrometry.

A compact device based on purge-and-trap multicapillary gas chromatography was developed for sensitive species-selective analysis of methylmercury and Hg2+ by atomic spectrometry. The operating mode includes in situ conversion of the analyte species to MeEtHg and HgEt2 and cryotrapping of the derivatives formed in a 0.53-mm-i.d. capillary, followed by their flash (< 30 s) isothermal low-temperature separation on a minimulticapillary (22 cm) column. The very low detection limits obtained (0.01 pg mL-1 of Hg for methylmercury) are due to the narrow injection band and reduced peak broadening in a bundle of 0.038-mm capillaries at high flow rates (> 60 mL min-1) compatible with an MIP AES detector (no dilution with a makeup gas is required). Developments regarding each of the steps of the analytical procedure and effects of operational variables (sample volume, purge flow, trap temperature, separation conditions) are discussed. The device allows speciation of MeHg+ and Hg2+ down to 5 pg g-1 in urine and, after a rapid microwave-assisted hydrolysis, down to 0.1 ng g-1 in solid biological samples with a throughput of 6 samples/h. The analytical protocols developed were validated by the analysis of DORM-1 (dogfish muscle), TORT-1 (lobster hepatopancreas), and Seronorm urine certified reference materials.

Animals↗