HPLC-MS/MS in der Rückstandsanalytik von Pflanzenschutzmitteln

Goal and Scope

Increasing demands from the regulatory authorities of plant protection products for residue analytical methods on the one hand and the need for cost reduction by shorter development times on the other hand have led to a significant displacement of conventional methods (e.g. HPLC-UV or GC-MS) by HPLC-MS/MS with atmospheric pressure ionization (API) in residue analysis since the mid of the 1990s. This development started in the pharmaceutical industries where HPLC-MS/MS had already been used for the quantitation of drugs and their metabolites in plasma since the late 1980s.

Methods

The reason for the high acceptability of HPLC-MS/MS with electrospray ionisation (ESI) or chemical ionization at atmosheric pressure (APCI) compared with alternative methods are shown with respect to analytical quality parameters, compliance with international registration guidelines and economic reasons.

Results and Conclusion

HPLC-MS/MS is being applied for solving ca. 75% of all analytical problems occuring in modern residue analytical laboratories. This technique offers convincing advantages for the determination of plant protection products and their metabolites in various matrices. These are a reduced number of or no clean-up steps after extraction of the samples, high throughput besides high ruggedness, low limits of detection and a large linear measuring range. In addition, several analytes of various chemical classes can be determined within one chromatographic run. Due to the high selectivity there is only little need for additional confirmatory methods. For enforcement purposes HPLC-MS/MS is accepted by the European authorities since 2002. However, due to high costs for instrumentation and specially skilled personnel only few enforcement laboratories have invested into this technology, so far.

Recommendation and Perspective

The importance of HPLC-MS/MS in residue analysis will further increase, as new ionization techniques will enable the analysis of more analytes and as the investment costs will decrease in the future. However, proven conventional methods will still survive in some cases. New concepts, such as parallel HPLC-MS/MS or on-line purification of extracts by column switching which are already widely used in the pharmaceutical industry could help to further increase the throughput. However, for a sound evaluation with respect to their applicability in residue analysis there is so far too little experience.     

Zur Entwicklung einer Prüfstrategie auf sexual-endokrine Wirksamkeit einer chemischen Substanz bei Fischen

Ohne Zusammenfassung Hintergrundinformation Umweltbundesamt (2007). Abschlussbericht des Forschungsprojektes „Charakterisierung endokrin vermittelter Wirkungen in Fischen: Relevante Parameter für die Entwicklung einer neuen OECD-Testmethode und in der Anwendung in der gesetzlichen Umweltrisikobewertung“ im Auftrag des Umweltbundesamtes (F?rderkennzeichen 206 67 470). Online erh?ltlich unter     

The construct validity of two burnout measures

The present study was carried out among a sample of 667 Dutch nurses and assesses three aspects of the construct validity of the two most widely used self-report burnout questionnaires: The Maslach Burnout Inventory (MBI) and the Burnout Measure (BM). Although the factorial validity of the three-dimensional structure of the MBI was convincingly demonstrated by confirmatory factor analysis with LISREL, four weak and ambiguous items were identified. Regarding the BM, some doubts have arisen about its one-dimensionality. The congruent validity of the questionnaires was well established: They both refer to the core element of the burnout syndrome (i.e. exhaustion). Moreover, linear structural analyses suggested that burnout is a two multi-dimensional construct consisting of an affective component (i.e. exhaustion) and an attitudinal component (i.e. a negative attitude towards recipients and towards one's job performance). However, the discriminant validity of the first component is rather poor since it considerably overlaps with self-reported somatic complaints and psychological strain. It is concluded that the MBI can be employed as a reliable and valid multi-dimensional indicator of burnout in professionals who work with people. The BM assesses the non-specific affective component of burnout (i.e. exhaustion) and should therefore be supplemented by a scale that measures the attitudinal component of the syndrome.     

Removing color and chlorinated organics from pulp mill bleach plant effluents by use of flyash

Color and chemical oxygen demand (COD) in bleach plant effluents are of concern. Acidified flyash can effectively remove both color and COD from caustic bleach plant effluents. Equally effective, but quicker and easier, is to acidify the effluent to approximately pH 1 and use untreated flyash. Based on maximum color removal, the required contact time is short, about 10 min, and the optimum ash dosage is that amount which raises the pH of the final effluent to about 5. Sufficient color removal is obtained to easily meet Maine's color regulations. Preliminary tests on samples of deionized water spiked with two arochlors of PCB showed high removal efficiency.The major cost of implementing and operating the cleanup procedure will be the cost of the required acid. This might be minimized by using some of the acidic (chlorine) effluent to lower the pH of the caustic effluent. This will, however, lead to less color reduction, and an unknown effect on the COD.     

Limit of safety against flame transmission for sintered metal flame arrester elements in the case of flashback in fuel gas/oxygen mixtures

In autogenous welding, cutting and allied processes, so-called dry safety devices are used to protect the outlet terminals of gas distribution lines. To prevent flame transmission, these units are fitted with sintered metal flame arrester elements. At the Federal Institute for Materials Research and Testing (BAM), extensive investigations have been carried out with an experimental flame arrester to determine the limits of safety against flame transmission for sintered metal flame arrester elements in the case of flashback in fuel gas/oxygen mixtures. On the basis of the results of these investigations, it is possible to estimate the pore sizes up to which a sintered metal element can prevent any flame transmission with a given fuel gas.     

N2O emissions from agricultural soils in the North China Plain:the effect of chemical nitrogen fertilizer and organic manure

ＩｎｔｒｏｄｕｃｔｉｏｎＮｉｔｒｏｕｓｏｘｉｄｅ (Ｎ2 Ｏ)ｉｓａｖｅｒｙｉｍｐｏｒｔａｎｔｇｒｅｅｎｈｏｕｓｅｇａｓｉｎｔｈｅａｔｍｏｓｐｈｅｒｅ.ＩｎｔｅｒｅｓｔｉｎｔｈｅｉｎｃｒｅａｓｅｏｆａｔｍｏｓｐｈｅｒｉｃＮ2 ＯｈａｓｂｅｅｎｒｅｃｅｎｔｌｙｓｔｉｍｕｌａｔｅｄｂｙｔｈｅｕｎｄｅｒｓｔａｎｄｉｎｇｔｈａｔＮ2 Ｏｇａｓｐｌａｙｓａｎｉｍｐｏｒｔａｎｔｒｏｌｅｉｎｔｈｅｃｈｅｍｉｓｔｒｙａｎｄｏｚｏｎｅｌａｙｅｒｄｅｓｔｒｕｃｔｉｏｎｏｆｔｈｅｓｔｒａｔｏｓｐｈｅｒｅ.Ｔｈｅｒａｄｉａｔｉｖ…     

Bacterioplankton Community Structure and Dynamics in Enclosures During Bioremediation Experiments in an Acid Mining Lake

In an acid mining lake (pH 2.6) enclosure experiments wereperformed with the addition of different concentrations oforganic carbon, nitrogen and phosphorus. SSCP-communityfingerprints, based on 16S rRNA gene amplicons, were performed tomonitor changes in the structure of the total bacterialcommunity and the sulfate reducing bacteria (SRB) in themesocosms. Total bacterial cell counts, as assessed byepifluorescence microscopy, were increased in the mesocosmsamended with organic carbon. The addition of carbon alsoincreased the number of abundant bacterial taxa substantiallyalong depth. Sulfate reducing bacteria (SRB) could be detected inall enclosures and all parts of the water column. These SRBbelonged to genus Desulfobacter as indicated bycoroborating molecular data.     

Die Wirkung von BaP und PCB 52 in gespikten Rieselfeldb?den auf das Wachstum vonAvena sativa (Hafer) undBrassica rapa (Stoppelrübe)

Ohne Zusammenfassung