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31.
Miège C Bouzige M Nicol S Dugay J Pichon V Hennion MC 《Journal of chromatography. A》1999,859(1):29-39
A selective clean-up procedure using immunoaffinity solid-phase extraction was applied for the trace-level determination of polycyclic aromatic hydrocarbons (PAHs) in urban waste water and sewage sludges used for soil amendment. Anti-pyrene antibodies have been immobilized on a silica-based sorbent and the cross-reactivity of the antibodies towards structurally related compounds were allowed to extract the whole class of priority PAHs. The selectivity of the antibodies provided clean extracts from sludges and, therefore, the identification and quantification were shown to be easier using either liquid chromatography (LC) with UV diode array and fluorescence detection in series or gas chromatography-mass spectrometry (GC-MS), although some loss of up to 50% was observed for the clean-up. The identification of the PAHs by matching of UV and MS spectra was greatly improved. The procedure, including immunoclean-up and LC coupled to diode array and fluorescence detection, was validated using certified reference materials with native PAHs of concentrations in the range of 0.57-2.16 mg/kg (dry sludges). 相似文献
32.
33.
Georges Machtalre Valrie Pichon Marie‐Claire Hennion 《Journal of separation science》2000,23(6):437-444
LC retention data have been measured using various stationary phases with an emphasis on highly polar to moderately polar neutral organic compounds having octanol‐water partition coefficients (Kow) in log units between 0 and 3. The relationships between the retention factor measured in water and the octanol‐water partition coefficient are linear but with different slopes for octadecyl (C18) silicas, and two polystyrene divinylbenzene (PS‐DVB) phases with low and high surface areas. These relationships confirm that highly cross‐linked polymers can provide more than 1000‐times higher retention values than C18 silicas for moderately polar analytes but close values for highly polar ones. They also explain why C18 silicas and polymers are equivalent for the separation of very polar analytes. In contrast, due to a different retention mechanism, no relation exists between the retention shown by porous graphitic carbons (PGC) and analyte hydrophobicity, but highly polar analytes are in general much more strongly retained than by any other sorbent. The potential of PGC for both the extraction and the separation of analytes is shown. Due to the difference in separation mechanism, PGC is the analytical phase that should be used for confirmation of the identity of analytes instead of a cyanopropylsilica column as recommended in some environmental procedures. Applications are presented for the trace‐determination of triazines and polar degradation products in ground and surface water with detection limits below the 0.1 μg/L level. 相似文献
34.
A new extraction immunosorbent involving antigen-antibody interactions was coupled on-line to liquid chromatography for the selective extraction in aqueous samples of benzidine and congeners, widely used as intermediate compounds in the manufacturing of dyes and pigments. Due to the cross-reactivity of the antibodies for analytes with chemical structures closely related to that of the analyte used for immunization, the immunoextraction sorbent was shown to be able to extract aminoazobenzene and related azo dyes with good recoveries. The on-line coupling was optimized for the trace determination of benzidine, dichlorobenzidine, aminoazobenzene and some azo dyes with detection limits in the range 0.1 to 1 microgram/l. The high selectivity of the immunoextraction was shown by comparing the analysis of an industrial textile effluent obtained using precolumns packed either with a non-selective polymeric sorbent or with the anti-benzidine immunosorbent. In such complex samples, extraction and clean-up are achieved in the same step. 相似文献
35.
Ferrocenyl sulfides afford meta-lithiation products with up to 94% regioselectivity on reaction with s-BuLi; the resulting 1,3-disubstituted ferrocenes can then be reacted with a variety of electrophiles. 相似文献
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37.
In this article we extend Milnor’s fibration theorem to the case of functions of the form with f, g holomorphic, defined on a complex analytic (possibly singular) germ (X, 0). We further refine this fibration theorem by looking not only at the link of , but also at its multi-link structure, which is more subtle. We mostly focus on the case when X has complex dimension two. Our main result (Theorem 4.4) gives in this case the equivalence of the following three statements:
Moreover one has that if these conditions hold, then the Milnor-Lê fibration of is a fibration of the multilink . We also give a combinatorial criterium to decide whether or not the multilink is fibered. If the meromorphic germ f/g is semitame, then we show that the Milnor-Lê fibration given by is equivalent to the usual Milnor fibration given by . We finish this article by discussing several realization problems.
Research partially supported by CONACYT and DGAPA-UNAM, Mexico, and by CNRS and ECOS, France. 相似文献
(i) | The real analytic germ has 0 as an isolated critical value; |
(ii) | the multilink is fibered; and |
(iii) | if is a resolution of the holomorphic germ , then for each rupture vertex (j) of the decorated dual graph of π one has that the corresponding multiplicities of f, g satisfy: . |
38.
An in-line procedure for protein analysis using a trypsin-based immobilized enzymatic reactor (IMER) coupled to LC-MS/MS has been developed. Various IMERs were synthesized and characterized by estimating the digestion yield of a pattern peptide in UV detection. Laboratory-made IMERs were optimized by studying the effect of different parameters as the nature of the functionalized immobilization support (silica, agarose), the amount of immobilized trypsin and the binding density. The potential of the laboratory-made IMERs were compared with a batch digestion and with a commercial trypsin-based IMER. The laboratory-made IMER based on CNBr-activated Sepharose showed the best performances in terms of digestion yields, digestion time, price and repeatability (RSD<4%). Cytochrome c was then digested on this IMER and used in-line with LC-MS. The target protein was easily recognized by the Mascot database until 17pmol injected. 相似文献
39.
Atrazine, desethyl-atrazine and desisopropyl-atrazine have been measured in the soils of Brévilles watershed. Pressurised liquid extraction (PLE) technique was used for extraction followed by purification with terbutylazine molecularly imprinted polymers. This clean-up procedure allowed to remove interfering compounds from the sample extracts. Thus making easier the analyses by reversed phase liquid chromatography coupled with ion trap tandem mass spectrometry. This selective sample treatment for soil extracts allowed limit of quantification (LOQ) of 0.03 ng/g for atrazine and 0.05 ng/g for metabolites. The concentrations in soil samples ranged from 7.1 ng/g to < LOQ for atrazine and from 2.5 ng/g to < LOQ for metabolites. The total cumulated mass in the top 60 cm of the soil of the watershed was estimated at 1.4, 0.52 and 0.25 kg for atrazine, desethyl-atrazine and desisopropyl-atrazine, respectively. A fraction of this mass available for leaching could generate water infiltrating with concentrations higher than the drinking water limit, 7 years after the last application of atrazine. 相似文献
40.
Ezzaher S Capon JF Gloaguen F Pétillon FY Schollhammer P Talarmin J Pichon R Kervarec N 《Inorganic chemistry》2007,46(9):3426-3428
Treatment of [Fe2(mu-pdt)(CO)6] [pdt=S(CH2)3S] with dppe (Ph2PCH2CH2PPh2) in refluxing toluene affords the asymmetric complex [Fe2(mu-pdt)(CO)4(dppe)] (1). Protonation of 1 with HBF4-Et2O in CH2Cl2 gives at room temperature the mu-hydrido derivative [Fe2(mu-pdt)(CO)4(dppe)(mu-H)](BF4) (2). Monitoring the reaction by 1H, 31P, and 13C NMR at low temperature reveals unambiguously that the process of the protonation of 1 implies terminal hydride intermediates. 相似文献