A liquid chromatographic (LC) multiresidue screening procedure was developed for determination of eprinomectin, moxidectin, abamectin, doramectin, and ivermectin in beef liver at 0, 25, 50, and 100 ppb levels. A procedure using low resolution LC/atmospheric pressure chemical ionization (APCI) mass spectrometry (MS) was developed with further purification steps added to the quantitative LC method to confirm residues. Acetonitrile extracts of liver, prior to derivatization for LC analysis, were further purified by using a C8 solid-phase extraction cartridge and an alumina-B cartridge. The purified extract was analyzed by injection into an LC/positive ion APCI MS. Identity of the compound was confirmed by comparison of its retention time and relative intensity data with those of a standard or recovery from a fortified control liver sample. Anthelmintic drugs in acetonitrile extracts of liver containing eprinomectin, moxidectin, abamectin, doramectin, and ivermectin at 25 ppb, the lowest level of fortification used in the LC determinative method, were successfully confirmed. 相似文献
Trimethyl (2S,3R)- and (2R,3R)-[2-2H1]-homocitrates, 10b and 10c respectively, and dimethyl (2S,3R)- and (2R,3R)-[2-2H1]-homocitric lactones, 11b and 11c respectively, have been synthesised from shikimic acid and [2-2H]-shikimic acid by a route which defines the stereochemistry of the two chiral centres in each compound. The NMR spectra of these products will enable the stereochemistry of the biological reaction catalysed by homocitrate synthase and by the protein from the nifV gene to be elucidated. 相似文献
Aliphatic and aromatic 1,3‐dithiane are oxidized to the corresponding carbonyl compounds in good yields under mild conditions by N,N′‐diiodo‐N,N′‐1,2‐ethanediyl‐bis(p‐toluenesulphonamide) [NIBTS] and silver nitrate. 相似文献
The polarographic behaviour of 1,3-bis[(2-pyridyl)methyleneamino]thiourea (PMAT) in solutions of varyingpH has been studied both in the absence and presence of Triton X-100 (T.X-100). The mechanism for the reduction process is discussed. The adsorption effect of electrochemically inactive T.X-100 on the polarographic waves ofPMAT has been investigated. The values of the kinetic parameters for the electrode reaction at differentpH values have been computed. The applicability of the polarographic method for determination ofPMAT is also discussed.
Das polarographische Verhalten von 1,3-Bis[(2-pyridyl)methylenamino]-thioharnstoff (PMAT) in Anwesenheit und Abwesenheit von Triton X-100. Die polarographische Bestimmung vonPMAT
Zusammenfassung Es wurde das polarographische Verhalten vonPMAT in Lösungen mit verschiedenempH sowohl in Gegenwart als auch ohne Triton X-100 (T.X-100) untersucht. Es wird ein Mechanismus für den Reduktionsprozeß diskutiert. Der Adsorptionseffekt des elektrochemisch inaktiven T.X-100 wurde hinsichtlich der polarographischen Wellen vonPMAT untersucht. Die kinetischen Parameter der Elektrodenreaktion wurden für verschiedenepH-Werte ermittelt. Ebenso wird die Anwendbarkeit der polarographischen Methode für die Bestimmung vonPMAT diskutiert.
The process of converting lignocellulosic biomass to ethanol via fermentation depends on developing economic sources of cellulases.Trichoderma reesei cellobiohydrolase (CBH) I is a key enzyme in the fungal cellulase system; however, specific process application requirements make modification of the enzyme by site-directed mutagenesis (SDM) an attractive goal. To undertake SDM investigations, an efficient, cellulase-free host is required. To test the potential ofEscherichia coli as a host, T.reesei CBH I cDNA was expressed inE. coli strain GI 724 as a C-terminal fusion to thermostable thioredoxin protein. Full-length expression of CBH I was subsequently verified by molecular weight, Western blot analysis, and activity on soluble substrates.
A new mercury(II) complex of 1,2‐bis(4‐pyridyle)ethene (bpe) with anionic acetate and thiocyanate ligands has been synthesized and characterized by elemental analysis, IR, 1H NMR and 13C NMR spectroscopy. The single crystal X‐ray analysis shows that the complex is a two‐dimensional polymer with simultaneously bridging 1,2‐bis(4‐pyridyle)ethane, acetate and thiocyanate ligands and basic repeating dimeric [Hg2(μ‐bpe)(μ‐OAc)2(μ‐SCN)2] units. The two‐dimensional system forms a three‐dimensional network by packing viaπ‐π stacking interactions. 相似文献
A simple and rapid microwave-assisted extraction (MAE) procedure was developed and optimized for the extraction of paclitaxel (Taxol) from the needles of yew trees Taxus baccata L. grown in Iranian habitats. The samples, immersed in a methanol-water mixture, were irradiated with microwaves in a closed-vessel system. The method was evaluated using a factorial design approach based on parameters such as extraction time, temperature, methanol concentration in water (v/v), and the ratio of grams of sample to 10 mL of solvent. Statistical treatment of the results revealed that the selected parameters were all significant except the extraction time. Optimum conditions would be 1.5 g samples in 10 mL solvent (90% methanol), an extraction temperature of 95 degrees C, and an extraction time of 7 min. The extracts has been analyzed by reverse-phase high-performance liquid chromatography with UV detection (LC/UV) at 227 nm for quantification. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) was used for confirmation. The main advantage of the proposed MAE method versus conventional solvent extraction (CSE) are the considerable reductions in time (7 min versus 16 h) and in solvent consumption (20 mL versus 150 mL). The MAE procedure yielded extracts that could be analyzed directly without any preliminary clean-up or solvent exchange steps. Both extraction methods show RSDs lower than 10% and lead to comparable recoveries of paclitaxel (87-92%). 相似文献
Dissociation equilibria of 4‐(2‐pyridylazo) resorcinol (PAR) in aqueous micellar solutions were determined spectrophotometrically at 25 °C and at the constant ionic strength I = 0.1 M KNO3. For this purpose, the effect of nonionic (Brij‐35, Triton X‐100, Triton X‐114, Triton X‐405), and anionic (SDS) surfactants on the absorption spectra of PAR at different pH values was studied. Results show that the pKa values and pure spectra of each species of PAR are influenced by percentages of a neutral and an anionic surfactant such as Brij‐35, Triton X‐100, Triton X‐114, Triton X‐405 and SDS, respectively, added to the solution of this reagent. 相似文献
The complexes formed by photosubstitution of pyrazine (Pz) in octacyanomolybdate(IV) and -tungstate(IV) with 8-hydroxyquinoline have been assigned the formulae [Mo(CN)2(OH)2(Pz)2(OX)] and [W(CN)2(OH)2(Pz)2(OX)·1.5H2O]. Coordination of Pz as an unidentate ligand by donating a lone pair of electron from nitrogen is shown by an absorption peak between 8–11 µ. Mechanism for the thermal decomposition of the complexes has been given. The formation of tungsten metal as residue in case of II has been confirmed by XRD analysis. The kinetic and thermodynamic parameters like activation energy (Ea), pre-exponential factor (A) and entropy of activation (S#) were calculated employing different integral methods of Doyle, Coats and Redfern and Arrhenius.H for each stage of decomposition was obtained from DSC.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献