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11.
A method has been developed for highly sensitive determination of haloperidol in human serum involving a simple extraction procedure followed by gas chromatographic separation. Target components were separated from the extracting solvents with a Van den Berg type solventless sample injector before introduction Into a DB-1 capillary separation column. A surface ionization detector (SID), which has highly selective sensitivity for Substituted amines, was employed for quantitation using bromperidol as an internal standard. Chloroform proved to be the best extracting solvent, yielding a quantitative detection limit of 5 ng/ml (S/N = 2). Comparison of the response to target compounds obtained by the SID, FTD (flame thermionic detector), and FID (flame ionization detector) showed the SID to be superior. 相似文献
12.
Determination of ofloxacin in human serum by high-performance liquid chromatography with column switching. 总被引:2,自引:0,他引:2
The chromatographic behaviour of ofloxacin on various sorbents, including ODS, C8, C1, nitril, phenyl and tert,-butyl, as stationary phases was investigated and a high-performance liquid chromatography (HPLC) assay was developed for the determination of ofloxacin in serum. The serum samples were directly introduced onto an HPLC column after filtering through a Morcut II membrane filter to remove proteins. The filtrate was concentrated on a pre-column using a phenyl stationary phase and was then introduced to an analytical column with an ODS stationary phase by column switching. Ofloxacin and enoxacin as an internal standard were detected by ultraviolet absorbance at 300 nm. Determination was possible for ofloxacin over the concentration range 50-2000 ng/ml; the limit of detection was 20 ng/ml. The recovery of ofloxacin added to serum was 88.8-101.7% with a coefficient of variation of less than 5.2%. This method is applicable to pharmacokinetic studies of patients after treatment with ofloxacin. 相似文献
13.
A supersonic jet instrument for fluorescence spectrometry is described. It consists of a high-temperature free expansion nozzle for continuous sample introduction and a vacuum chamber equipped with a high-speed pumping system. Rotationally cooled spectra obtained with the supersonic jet are compared with gas-phase spectra measured at high temperature for perylene and benzo[a]pyrene molecules. Each component of the unresolved band structure in the high-temperature spectra was found to be composed of a rotational congestion of several vibrational bands. For a 1:1 mixture of perylene and benzo[a]pyrene, selective detection is possible by using supersonic jet spectrometry. The detection limit for perylene is 100 ng. The advantage of this technique over other low-temperature spectrometric methods based on Shpol'skii and matrix isolation effects are discussed. 相似文献
14.
A method of rapid determination for indium, nickel and copper in Spinach (NBS; SRM-1570) by substoichiometric radioactivation
analysis is described. The method is based on the principle that an equal amount of non-irradiated test sample is added to
the irradiated standard sample and subsequent substoichiometric extraction for the irradiated test and standard samples is
carried out. Indium is extracted as diethyldithiocarbamate into carbon tetrachloride, nickel as dimethylglyoximate into chloroform
and copper as dithizonate into carbon tetrachloride. The radioactivities of these extracts are measured by NaI(Tl) or Ge(Li)
detector coupled with pulse-height analyser. The analytical results obtained by the method were in good agreement with our
published values and certified values by NBS. 相似文献
15.
16.
Fujii H Hirano N Uchiro H Kawamura K Nagase H 《Chemical & pharmaceutical bulletin》2004,52(6):747-750
7beta-Carbamoyl-4,5alpha-epoxymorphinans 5 were stereoselectively synthesized from the 7alpha-carboxylate intermediate 3 in the presence of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) and amines under reflux conditions in mesitylene via a novel and reactive gamma-lactone 7. These were the first examples of the stereoselective syntheses of 7beta-substituted 4,5alpha-epoxymorphinans. The mechanism of the reaction process was elucidated as follows: 1) epimerization of 7alpha-carboxylate 3, 2) intramolecular lactonization of 7beta-carboxylate 6, and 3) aminolysis of the resultant gamma-lactone 7. The aminolysis of the isolated reactive gamma-lactone 7 with allylamine and the alcoholysis with MeOH in the presence of NaBH(4) proceeded at room temperature. The gamma-lactone 7 can be a useful intermediate for the preparation of 7beta-substituted 4,5alpha-epoxymorphinans that would be potent selective delta opioid receptor ligands. The stereoselective syntheses of the 7alpha-carbamoyl-4,5alpha-epoxymorphinans 9 from 7alpha-carboxylate 3 via 7alpha-carboxylic acid were also successful. 相似文献
17.
A study of the substoichiometric extraction of phosphorus is described. Phosphorus was extracted in the form of ternary compounds
such as ammonium phosphomolybdate, 8-hydroxyquinolinium phosphomolybdate, tetraphenylarsonium phosphomolybdate and tri-n-octylamine
phosphomolybdate. Consequently, phosphorus was extracted substoichiometrically by the addition of a substoichiometric amount
of molybdenum for all four phosphomolybdate compounds. On the other hand, phosphorus could be separated substoichiometrically
with a substoichiometric amount of tetraphenylarsonium chloride or tri-n-octylamine. Stoichiometric ratios of these ternary
compounds obtained substoichiometrically were 1∶12∶3 for phosphorus, molybdenum and organic reagent. Applicability of these
compounds to phosphorus determination was also discussed. 相似文献
18.
Commercially available powdered photocatalysts such as P-25 are known to show high photocatalytic performance. However, in practical use, their anchoring onto a substrate without any binders is still very difficult. The purpose of this study is to design and develop high-performance photocatalysts that can be anchored onto a substrate, and to this end we have prepared a titanium oxide photocatalyst using a wet process. The results of this study led to the successful development of rectangular column structured titanium oxide crystals which could be anchored onto silica sheets. The rectangular columnar crystal was 100- 500 nm wide and 1000- 5000 nm long. Moreover, investigations on the complete oxidation reaction of acetaldehyde into CO2 and H2O showed a high performance equivalent to that of the most efficient marketed powdered photocatalysts. 相似文献
19.
Phosphorus in orchard leaves (NBS SRM-1571) and spinach (SRM-1570) was determined by various substoichiometric analytical
methods such as the direct method, GRASHCHENKO's method and the method of carrier amount variation. All samples were labelled
with32P radioisotope. The data obtained by the method of carrier amount variation were also treated by the method of least squares
instead of De VOE's method. Phosphorus concentration in orchard leaves was 0.206±0.011% by the direct method, 0.219±0.011%
by GRASHCHENKO's method, 0.211±0.011% by the method of carrier amount variation and 0.207±0.007% by the method of least squares,
respectively. These values agree with the value reported by NBS (0.21±0.01%). Furthermore, these concentrations obtained by
various substoichiometric methods were compared with those by radioactivation reported in a prevoius paper. 相似文献
20.
Dobashi T Nobe M Yoshihara H Yamamoto T Konno A 《Langmuir : the ACS journal of surfaces and colloids》2004,20(16):6530-6534
Curdlan dissolved in aqueous sodium hydroxide was dialyzed to aqueous calcium chloride to form a gel. Transparent and turbid concentric layers observed in the gel cross section perpendicular to the long axis of the dialysis tube were identified as liquid crystalline gels with refractive index gradient and amorphous gels, respectively. The thickness of each layer was proportional to the diameter of the dialysis tube, and the gelation proceeded in proportion to the root of time. The unique pattern formation was attributed to the change of curdlan conformation and calcium-induced cross-linking resulting from a diffusion of calcium cations and hydroxide anions through the dialysis tube. It is suggested that the orderedness of the curdlan molecules decreases by the increase of the curvature of the concentric liquid crystal layers as the layer comes toward the center of the dialysis tube. 相似文献