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21.
Evaluation of gas chromatography-tandem quadrupole mass spectrometry for the determination of organochlorine pesticides in fats and oils 总被引:1,自引:0,他引:1
Patel K Fussell RJ Hetmanski M Goodall DM Keely BJ 《Journal of chromatography. A》2005,1068(2):289-296
A gas chromatography-tandem quadrupole mass spectrometry multi-residue method for the analysis of 19 organochlorine pesticides in fats and oils has been developed. Gel permeation chromatography was employed to remove lipid material prior to GC-MS/MS analysis. Average recoveries of the pesticides spiked at 10 and 50 microg kg(-1) into fish oil, pork fat, olive oil and hydrogenated vegetable oil were typically in the range 70-110% with relative standard deviations generally less than 10%. Calculated limits of detection are between 0.1 and 2.0 microg kg(-1) and results obtained for the analysis of proficiency test materials are in good agreement with assigned values. The higher selectivity of the GC-MS/MS compared to electron capture detection and GC-MS in selective ion monitoring mode allowed unambiguous identification and confirmation of all the target pesticides at low microg kg(-1) levels in fats and oils in a single analysis. 相似文献
22.
Appleby I Boulton LT Cobley CJ Hill C Hughes ML de Koning PD Lennon IC Praquin C Ramsden JA Samuel HJ Willis N 《Organic letters》2005,7(10):1931-1934
Two methods to produce (2S)-5-amino-2-(1-n-propyl-1H-imidazol-4-ylmethyl)-pentanoic acid were investigated. Diastereoisomeric salt resolution, using the quinidine salt, gave the desired intermediate in 98% ee and 33% yield. Asymmetric hydrogenation of various substrates gave high conversions, with up to 83% ee. Integration of these two approaches via asymmetric hydrogenation of a quinidine salt substrate followed by crystallization provided the desired intermediate in 94% ee and 76% yield. 相似文献
23.
24.
Applied Biochemistry and Biotechnology - 相似文献
25.
The structure of the complex, [Fe2(II)Fe2(III)(HCOO)10(C6H7N6)n, (1) exhibits a neutral two-dimensional layer network of alternating iron(II) and iron(III) ions, bridged equatorially by formate groups. All iron atoms are octahedrally coordinated, with iron(III) coordinating axially to one gamma-picoline and one formate group, while the iron(II) centers interact axially with two gamma-picoline groups, above and below the layer plane. The complex crystallizes in the triclinic space group P1 at all studied temperatures [at 120 K, the cell dimensions are: a = 10.228(1), b = 12.071(1), c = 12.072(1) A, alpha = 89.801(2), beta = 71.149(2), gamma = 73.371(2) degrees]. An intralayer antiferromagnetic exchange interaction of J = -2.8 cm(-1) between iron(II) and iron(III) was observed in the magnetic studies. Decreasing the temperature to close to 20 K causes a magnetic-ordering phenomenon to occur and a low-temperature phase with a long-range antiferromagnetic spin orientation appears. The magnetic phase transition was confirmed by M?ssbauer spectroscopic studies at temperatures above and below the critical temperature. Structural information of 1 from synchrotron X-ray diffraction data collected at room temperature and 16 K suggests that the antiferromagnetic ordering is caused by an enhanced pi-pi interaction between chi-picoline groups from adjacent layers. 相似文献
26.
Abdul Majid Jim Tunney Steve Argue Mike Post 《Journal of Sol-Gel Science and Technology》2004,32(1-3):323-326
We have investigated the synthesis of perovskite-type SrFeOx (2.5 x 3.0) using three preparative methods: sol-gel, mechanochemical processing and solid state reactions at high temperature of the corresponding oxides. The sample obtained after calcination of the gel from sol-gel method, contained the least amount of strontium carbonate impurity. The amount of strontium carbonate impurity decreased with the increase in calcination temperature. Perovskites obtained have been characterized by X-ray diffraction (XRD) and nitrogen adsorption isotherms. Samples obtained from three methods have been compared with respect to calcination temperature, crystallite size and specific surface area.Issued as NRCC No. 46479. 相似文献
27.
Yan B Collins N Wheatley J Irving M Leopold K Chan C Shornikov A Fang L Lee A Stock M Zhao J 《Journal of combinatorial chemistry》2004,6(2):255-261
We have developed a high-throughput purification system to purify combinatorial libraries at a 50-100-mg scale with a throughput of 250 samples/instrument/day. We applied an accelerated retention window method to shorten the purification time and targeted one fraction per injection to simplify data tracking, lower QC workload, and simplify the postpurification processing. First, we determined the accurate retention time and peak height for all compounds using an eight-channel parallel LC/UV/MS system, and calculated the specific preparative HPLC conditions for individual compounds. The preparative HPLC conditions include the compound-specific gradient segment for individual compounds with a fixed gradient slope and the compound-specific UV or ELSD threshold for triggering a fraction collection device. A unique solvent composition or solvent strength was programmed for each compound in the preparative HPLC in order to elute all compounds at the same target time. Considering the possible deviation of the predicted retention time, a 1-min window around the target time was set to collect peaks above a threshold based on UV or ELSD detection. Dual column preparative instruments were used to maximize throughput. We have purified more than 500 000 druglike compounds using this system in the past 3 years. We report various components of this high-throughput purification system and some of our purification results. 相似文献
28.
Changes in the mass spectra with inlet temperature were used in this work to demonstrate the dependence of keto-enol tautomerism of acetylacetone, 3-methyl acetylacetone and 3-allyl acetylacetone on temperature. The largest dependence of temperature were shown by the ion [M ? 42]+. arising from a McLafferty type rearrangement and by the ion [M ? Me]+ resulting from simple α-cleavage. The ion [M ? 42]+. peak increases with the temperature of the inlet system while the ion [M ? Me]+ peak decreases. By assuming that the ion [M ? 42]+. represents the keto form and that the ion [M ? Me]+ represents the cis-enol form (stabilized by the hydrogen bond) one sees that the direction of the intensity variation of these peaks with temperature is in accord with the expected change of keto-enol tautomerism with temperature. A quantitative correlation on the basis of the above assumptions is also approached. Recording of the mass spectra of these three β-diketones at different energies of the incident electrons enables us to estimate whether or not the particular ions present in the mass spectra result from energetically favourable processes. The variation of the intensities of the peaks with the temperature of the inlet at different electron energies is also discussed. 相似文献
29.
Ian K. Boddy J. Boniface Richard C. Cambie Peter A. Craw David S. Larsen Hamish McDonald Peter S. Rutledge Paul D. Woodgate 《Tetrahedron letters》1982,23(42):4407-4408
Gentle heating of allyloxyanthraquinones with sodium dithionite in dimethylformanide - water effects a rapid and controlled rearrangement to give high yields of 2-allyanthraquinones. 相似文献
30.
Klein SR Himel TM Abrams G Amidei D Baden AR Barklow T Boyarski AM Boyer J Burchat PR Burke DL Butler F Dorfan JM Feldman GJ Gidal G Gladney L Gold MS Goldhaber G Golding L Haggerty J Hanson G Hayes K Herrup D Hollebeek RJ Innes WR Jaros JA Juricic I Kadyk JA Karlen D Lankford AJ Larsen RR LeClaire BW Levi M Lockyer NS Lüth V Matteuzzi C Nelson ME Ong RA Perl ML Petersen A Richter B Riles K Rowson PC Schaad T Schellman H Schmidke WB Sheldon PD Trilling GH de la Vaissiere C Wood DR Yelton JM 《Physical review letters》1987,58(7):644-647