Journal of Mass Spectrometry | Year: 2012
This study investigates to which extent the design of electrospray ion sources influences the susceptibility to matrix effects (MEs) in liquid chromatography-tandem mass spectrometry (LC-MS/MS). For this purpose, MEs were measured under comparable conditions (identical sample extracts, identical LC column, same chromatographic method and always positive ion mode) on four LC-MS/MS instrument platforms. The instruments were combined with five electrospray ion sources, viz. Turbo Ion Spray, Turbo VTM Source, Standard ESI, Jet Stream ESI and Standard Z-Spray Source. The comparison of MEs could be made at all retention times because the method of permanent postcolumn infusion was applied. The MEs ascertained for 45 pesticides showed for each electrospray ion source the same pattern, i.e. the same number of characteristic signal suppressions at equivalent retention times in the chromatogram. The Turbo Ion Spray (off-axis geometry), Turbo VTM Source (orthogonal geometry) and the Standard Z-Spray Source (double orthogonal geometry) did not differ much in their susceptibility to MEs. The Jet Stream ESI (orthogonal geometry) reaches a higher sensitivity by an additional heated sheath gas, but suffers at the same time from significantly stronger signal suppressions than the comparable Standard ESI (orthogonal geometry) without sheath gas. No relation between source geometry and extent of signal suppression was found in this study. Copyright © 2012 John Wiley & Sons, Ltd.
Forster A.,German Research Center for Geosciences |
Schoner R.,Friedrich - Schiller University of Jena |
Forster H.J.,German Research Center for Geosciences |
Norden B.,German Research Center for Geosciences |
And 5 more authors.
Marine and Petroleum Geology | Year: 2010
Ketzin, in the Northeast German Basin (NEGB), is the site for pilot injection of CO2 (CO2SINK project) into a saline aquifer (the Upper Triassic Stuttgart Formation) situated at a depth of about 630-700m. This paper reports the baseline characterization of the reservoir formation based on new core material and well-logs obtained from one injection well and two observations wells, drilled at a distance from 50m to 100m from each other. The reservoir is lithologically heterogeneous and made up by fluvial sandstones and siltstones interbedded with mudstones showing remarkable differences in porosity. The thickest sandstone units are associated with channel sandstone, whose thickness varies over short lateral distances. In-depth petrographic, mineralogical, mineral-chemical, and whole-rock geochemical analysis were performed focusing on the sandstone intervals, which display the best reservoir properties for CO2 injection. The dominantly fine-grained and well to moderately-well sorted, immature sandstones classify as feldspathic litharenites and lithic arkoses. Quartz (22-43wt.%), plagioclase (19-32wt.%), and K-feldspar (5-13wt.%) predominate mineralogically. Muscovite plus illite and mixed-layer minerals are omnipresent (4-13wt.%). Quartz, feldspar, as well as meta-sedimentary and volcanic rock fragments comprise the most abundant detrital components, which often are rimmed by thin, early diagenetic coatings of ferric oxides, and locally of clay minerals. Feldspar grains may be unaltered and optically clear, partially to completely dissolved, partially altered to sheet silicates (mainly illite), or albitized. Analcime and anhydrite constitute the most widespread, often spatially associated pore-filling cement minerals. Authigenic dolomite, barite, and coelestine is minor. The percentage of cements ranges in total from about 5vol.% to 32vol.%. Except of samples intensely cemented by anhydrite and analcime, total porosities of the sandstones range from 13% to 26%. The fraction of intergranular porosity varies between 12% and 21%. About 1-5% porosity has been generated by dissolution of detrital plagioclase, K-feldspar, and volcanic rock fragments. The comparatively large modal abundance of feldspars, micas, chlorite, clay minerals, Fe-Ti-oxides, and analcime account for the richness in Ti, Al, Fe, Mg, Na, and K, and the paucity in Si, of the Stuttgart sandstones relative to mature sandstones. Altogether, these sandstones are comparatively rich in minerals that may potentially react with the injected CO2. © 2010 Elsevier Ltd.
SUMMARY A total of 2475 animals from Germany, both captive and wild, were tested for antibodies against Francisella tularensis to obtain more knowledge about the presence of this pathogen in Germany. An indirect and a competitive ELISA served as screening methods, positive and inconclusive samples were confirmed by Western blot. Of the zoo animals sampled between 1992 and 2007 (nÂ =Â 1122), three (0.3%) were seropositive. The seroconversion of a hippopotamus in Berlin Zoo was documented. From 1353 serum samples of wild foxes (Vulpes vulpes), raccoon dogs (Nyctereutes procyonoides) and wild boars (Sus scrofa), collected between 2005 and 2009 in the federal state of Brandenburg (surrounding Berlin), a total of 101 (7.5%) tested positive for antibodies to F. tularensis lipopolysaccharide. Our results indicate a higher seroprevalence of F. tularensis in wildlife in eastern Germany than commonly assumed. Furthermore, we found foxes and raccoon dogs to be biological indicators for tularaemia. Copyright © Cambridge University Press 2012.
Dirofilaria repens is endemic in eastern and southern European regions but was recently found in Germany in dogs, mosquitoes and one human patient. Since some of the positive dog and mosquito samples were collected in Brandenburg, it was aimed to systematically assess the prevalence of D. repens and other canine vector-borne pathogens in Brandenburg. Dog owners also received a questionnaire and were asked to provide more information about the dogs including travel history. In total, 1023 dog blood samples as well as 195 fox spleen and 179 fox blood samples were collected. DNA was analysed by PCR for the presence of filariae, piroplasms, anaplasmataceae and Rickettsia spp. Filariae were detected in six dogs (0.6%), two were positive for DNA from D. repens, two from Dirofilaria immitis and two from Acanthocheilonema reconditum. One of the D. repens positive dogs originated from an animal shelter in Brandenburg, but the origin of the other one remained unknown. Interestingly, both D. repens ITS-1 sequences showed 100% identity to a D. repens sample obtained from a Japanese woman that travelled in Europe and were 97% identical to a newly proposed species Dirofilaria sp. hongkongensis described from Hong Kong. However, identity to other D. repens sequences from Thailand was considerably lower (81%). Identity of 12S rRNA and cytochrome oxidase I to D. repens samples from southern Europe was 99%. Due to the low number of Dirofilaria spp. positive dogs and since the origin of these was unknown, endemic occurrence of Dirofilaria in Brandenburg could not be confirmed. Anaplasma phagocytophilum was found in 15 dogs (1.5%), Candidatus Neoehrlichia mikurensis in three dogs (0.3%) and E. canis in one dog (0.1%), which was co-infected with D. repens. Rickettsia spp. were detected in 8 dogs (0.8%), seven were Rickettsia raoultii and one was Rickettsia felis. To the authors knowledge, R. raoultii DNA was detected for the first time in dogs in Germany in this study and Candidatus N. mikurensis for the second time. In spleen samples of red foxes with 47.5% a high prevalence of piroplasms was found. Sequencing of 11 samples identified 10 as Theileria annae. Despite the high prevalence of this pathogen in its reservoir host, it was absent in dog samples. In one dog (0.1%), Babesia canis was detected but there was no further information about the dogs origin. Evaluation of the questionnaire identified a high proportion of dogs (74.2%, n=233) which was not protected by ectoparasiticides. Moreover, 21.2% (n=236) of the dogs originated from inland or abroad shelters, and therefore might potentially come from areas endemic for dirofilariosis or babesiosis.
Rapid and simple determination of residues of the aniline-forming pesticides amitraz, vinclozolin and chlorpropham in plant-based foodstuffs and honey by means of HS-SPME and GC-MS according to residue definition [Schnelle und einfache Rückstandsbestimmung der anilinbildenden Pflanzenschutzmittel Amitraz, Vinclozolin und Chlorpropham in pflanzlichen Lebensmitteln und Honig durch HS-SPME und GC-MS gemäß Rückstandsdefinition]
We describe development and validation of a method, which allows the determination of the total residues of the pesticides Amitraz, Vinclozolin, and Chorpropham, including their degradation products as required by the definition of residues, in phytogenic foodstuffs and honey. The effort in terms of work force and equipment needed to carry out these measurements is extremely small. The standard procedures based on steam distillation were replaced by performing the hydrolysis in a screws head-space vial overnight in a drying oven at 90°C. The extraction is carried out by headspace solid-phase extraction at 60°C for 30 min. Desorption happens in the injector of the gas Chromatograph. As detector any MSD or a GC-MS-MS are suitable. The method tested using pear, potato, kiwi, and honey matrices. The procedure shows a very good linearity for all four analytes over the range 10-2000 µg/kg, it is therefore perfectly suited for monitoring the statutory maximum levels. The recovery rates amounted to 88-100 [%] for adding 50 µg/kg to a pear matrix. The relative standard deviation of the measured values was 5-18 [%] with the MSD and 2-6 [%] with the GC-MS-MS. In diesem Beitrag kann nur eine Abbildung gezeigt werden. Weitere Chromatogramme (Kartoffel, Kiwi, Birne und Honig) können jedoch beim Autor eingesehen werden.