Use of micellar mobile phases for the chromatographic determination of melamine in dietetic supplements

Melamine is a nitrogen-rich industrial chemical which is occasionally used to increase the apparent protein content of different products destined for human and animal consumption. In this work, a liquid chromatographic procedure that uses micellar mobile phases of sodium dodecyl sulfate (SDS) buffered at pH 3, a C18 column and UV detection is reported for the determination of melamine in dietetic supplements. Samples were reconstituted with a SDS solution and were directly injected, thus avoiding long extraction and experimental procedures. Melamine was eluted in less than 10 min with no interference by other compounds of the matrices. The optimum mobile phase composition was taken by a chemometrical approach that considers the retention factor, efficiency and peak shape. Validation was performed following the indications of the European Commission (Decision 2002/657/EC). The following parameters were considered: linearity (0.02-100 μg mL(-1); R(2) = 0.9996), intra- and inter-day precisions (<12.4%), accuracy (90.0-101.3%), and robustness (less than 9.8% and 5.1%, for retention time and peak area, respectively). The limits of detection and quantification were 9 and 20 ng mL(-1), respectively. Recoveries for several spiked samples were in the 85.8-114.3% range. These results indicate that the proposed methodology is useful for routine analysis of control quality of infant formula and adult dietetic supplement

Hi-GAL, theHerschelinfrared Galactic Plane Survey: photometric maps and compact source catalogues

Aims. We present the first public release of high-quality data products (DR1) from Hi-GAL, the Herschel infrared Galactic Plane Survey. Hi-GAL is the keystone of a suite of continuum Galactic plane surveys from the near-IR to the radio and covers five wavebands at 70, 160, 250, 350 and 500 µm, encompassing the peak of the spectral energy distribution of cold dust for 8 < T < 50 K. This first Hi-GAL data release covers the inner Milky Way in the longitude range 68◦ > t > −70◦ in a |b| ≤ 1◦ latitude strip. ∼ ∼ ∼ ∼ Methods. Photometric maps have been produced with the ROMAGAL pipeline, which optimally capitalizes on the excellent sensitivity and stability of the bolometer arrays of the Herschel PACS and SPIRE photometric cameras. It delivers images of exquisite quality and dynamical range, absolutely calibrated with Planck and IRAS, and recovers extended emission at all wavelengths and all spatial scales, from the point-spread function to the size of an entire 2◦ × 2◦ “tile” that is the unit observing block of the survey. The compact source catalogues were generated with the CuTEx algorithm, which was specifically developed to optimise source detection and extraction in the extreme conditions of intense and spatially varying background that are found in the Galactic plane in the thermal infrared. Results. Hi-GAL DR1 images are cirrus noise limited and reach the 1σ-rms predicted by the Herschel Time Estimators for parallel-mode obser- vations at 6011 s−1 scanning speed in relatively low cirrus emission regions. Hi-GAL DR1 images will be accessible through a dedicated web-based image cutout service. The DR1 Compact Source Catalogues are delivered as single-band photometric lists containing, in addition to source posi- tion, peak, and integrated flux and source sizes, a variety of parameters useful to assess the quality and reliability of the extracted sources. Caveats and hints to help in this assessment are provided. Flux completeness limits in all bands are determined from extensive synthetic source experiments and greatly depend on the specific line of sight along the Galactic plane because the background strongly varies as a function of Galactic longitude. Hi-GAL DR1 catalogues contain 123210, 308509, 280685, 160972, and 85460 compact sources in the five bands

The Hi-GAL compact source catalogue – I. The physical properties of the clumps in the inner Galaxy (−71. ◦ 0 < ℓ < 67.◦ 0)

Hi-GAL (Herschel InfraRed Galactic Plane Survey) is a large-scale survey of the Galactic plane, performed with Herschel in five infrared continuum bands between 70 and 500 µm. We present a band-merged catalogue of spatially matched sources and their properties derived from fits to the spectral energy distributions (SEDs) and heliocentric distances, based on the photometric catalogues presented in Molinari et al., covering the portion of Galactic plane −71.◦ 0 < ℓ < 67.◦ 0. The band-merged catalogue contains 100 922 sources with a regular SED, 24 584 of which show a 70-µm counterpart and are thus considered protostellar, while the remainder are considered starless. Thanks to this huge number of sources, we are able to carry out a preliminary analysis of early stages of star formation, identifying the conditions that characterize different evolutionary phases on a statistically significant basis. We calculate surface densities to investigate the gravitational stability of clumps and their potential to form massive stars. We also explore evolutionary status metrics such as the dust temperature, luminosity and bolometric temperature, finding that these are higher in protostellar sources compared to pre-stellar ones. The surface density of sources follows an increasing trend as they evolve from pre-stellar to protostellar, but then it is found to decrease again in the majority of the most evolved clumps. Finally, we study the physical parameters of sources with respect to Galactic longitude and the association with spiral arms, finding only minor or no differences between the average evolutionary status of sources in the fourth and first Galactic quadrants, or between 'on-arm' and 'interarm' positions

Development and validation of a micellar liquid chromatography-based method to quantify melamine in swine kidney

Melamine is a toxic compound illegally added to animal feed to falsely boost protein content. This represents a strong threat to consumer's health, as melamine can reach human through the food chain. An easy and reliable micellar liquid chromatography-method was developed to detect melamine in swine kidney. The analyte was extracted by shaking in methanol. Melamine was eluted from the HPLC column without interferences in 0.9997), precision (<7.6%), accuracy (−8.3–3.6%), recovery (82.1–92.4%) and robustness (<5.1%). The methodology was applied to swine kidney samples purchased from a local supermarket. The method can be used as a screening method for routine post-mortem diagnose melamine intoxication in animals and detect feeding with poultry containing melamine, in order to withdraw the corresponding flesh. This would be mandatory to prevent consumer intoxication and improve the quality of food

Validation of an analytical methodology to quantify melamine in body fluids using micellar liquid chromatography

Measurement of urine and plasma melamine-concentration is helpful in confirming melamine-associated renal diseases. A chromatographic procedure using a C18 column and a micellar mobile phase of sodium dodecyl sulphate (0.2 M), buffered at pH 3 and detection set at 210 nm, was reported for the resolution and quantification of melamine in plasma and urine. In this work, direct injection was used, thus avoiding long extraction and experimental procedures. Melamine was eluted in nearly 6.3 min without overlapping the protein band or other endogenous compounds. The optimal mobile phase composition was taken by studying the influence of each chromatographic parameter. Validation was satisfactorily performed following the US Food and Drug Administration (FDA), in terms of: linearity (0.25–25 ppm; r2 > 0.9995 in both cases), sensitivity, limit of detection (50 ppb), limit of quantification (250 ppb), intra- and inter-day precision (R.S.D. 0.7–10.2% and 1.0–9.1%, respectively) and recovery, calculated as accuracy (85.7–103.8% and 94.8–103.6%, respectively) and robustness (R.S.D. < 7.1%). The suggested methodology has been applied to the analysis of real samples of volunteers, and no melamine was found in any of them

Development of an analytical methodology to quantify melamine in milk using micellar liquid chromatography and validation according to EU Regulation 2002/654/EC

Melamine is a toxic triazine, illegally used as an additive in milk to apparently increase the amount of protein. A chromatographic procedure using a C18 column and a micellar mobile phase of sodium dodecyl sulphate (0.05 M) and propanol (7.5%), buffered at pH 3, and a detection set by absorbance at 210 nm, was reported for the resolution and quantification of melamine in liquid and powdered milk samples. In this work, samples were diluted with a SDS solution and were directly injected, thus avoiding long extraction and experimental procedures. Melamine was eluted in nearly 9.3 min without overlapping the protein band or other endogeneous compounds. The optimal mobile phase composition was taken using a chemometrical approach that considers the retention factor, efficiency and peak shape. Validation was performed following the European Commission's indications (European Decision 2002/657/EC), and the main analytical parameters studied were: linearity (0.02-100 ppm; r2 = 0.999), limit of detection (5 ppb), intra- and inter-day precision (R.S.D. &lt;7.6% and &lt;9.7%, respectively) and robustness (R.S.D. &lt;7.4% for retention time and &lt;5.0% for area). Sensitivity was adequate to detect melamine under the safety limits proposed by the US FDA. Finally, recoveries for several milk samples were found in the 85-109% range. © 2010 Elsevier B.V. All rights reserved

Quantification of Melamine in Drinking Water and Wastewater by Micellar Liquid Chromatography

Because of the large potential health impact caused by deliberate contamination with the synthetic chemical melamine of different products for human and animal consumption, the World Health Organization and the Food and Agriculture Organization of the United Nations provided a range of recommendations in order to facilitate obtaining needed data, among which was the determination of the background levels of melamine in drinking water and wastewater (December 4, 2008). A chromatographic procedure using a C18 column, a micellar mobile phase consisting of sodium dodecyl sulfate (0.1 M), and 1-propanol (7.5%) buffered at pH 3, and detection by absorbance at 210 nm is reported in this paper for the quantification of melamine in drinking water and wastewater. Samples were filtered and directly injected into the chromatographic system, thus avoiding an extraction procedure. The optimal mobile phase composition was obtained by a chemometrics approach that considered the retention factor, efficiency, and peak shape. Melamine was eluted in about 6.2 min without interferences. Validation was performed following U.S. Food and Drug Administration guidelines. The analytical parameters studied were linearity (0.03–5 μg/mL, R2 = 0.998), LOD (13 ng/mL), intraday and interday accuracy (between 4.1 and 12.2%), intraday and interday precision (less than 14.8%), and robustness (RSD < 5.1% for retention time and <9.0% for area). The proposed methodology was successfully applied for analysis of local wastewater and drinking water, in which no melamine was found

Analytical determination of hydroxytyrosol in olive extract samples by micellar liquid chromatography

Hydroxytyrosol is a well-known natural phenolic component obtained from olive extract samples with antioxidant effects. A micellar liquid chromatography method to detect and quantify hydroxytyrosol in olive extract samples is described. Matrix resolution was performed using a Kromasil C18 column and a micellar mobile phase of sodium dodecyl sulphate (SDS) 0.05 M and 4% methanol buffered at pH 7. Detection was set by absorbance at 280 nm. Samples were diluted with 0.05 M SDS at pH 3 and directly injected, thus avoiding long tedious extractions. Hydroxytyrosol was eluted in 3.5 min without overlapping other matrix compounds. Validation was performed following the US FDA guideline. The main analytical parameters studied were: linearity (0.03–250 μg mL−1; r2 = 0.999), limit of detection and quantification (3 and 30 ng mL−1, respectively), intra- and inter-day precision (RSD, % <1.4 and <8.2, respectively), and robustness (RSD, % < 6.6). Recoveries were in the 88.5–98.9% range