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51.
Roman MC 《Journal of AOAC International》2004,87(1):1-14
An international collaborative study was conducted of a high-performance liquid chromatography (HPLC)-UV method for the determination of the major (ephedrine [EP] and pseudoephedrine [PS]) and minor (norephedrine [NE], norpseudoephedrine [NP], methylephedrine [ME], and methylpseudoephedrine [MP]) alkaloids in selected dietary supplements representative of the commercially available products. Ten collaborating laboratories determined the ephedrine-type alkaloid content in 8 blind replicate samples. Five products contained ephedra ground herb or ephedra extract. These 5 products included ground botanical raw material of Ephedra sinica, a common powdered extract of Ephedra sinica, a finished product containing only Ephedra sinica ground botanical raw material, a complex multicomponent dietary supplement containing Ma Huang, and a high-protein chocolate flavored drink mix containing Ma Huang extract. In addition, collaborating laboratories received a negative control and negative control spiked with ephedrine alkaloids at high and low levels for recovery studies. Test extracts were treated to solid-phase extraction using a strong-cation exchange column to help remove interferences. The HPLC analyses were performed on a polar-embedded phenyl column using UV detection at 210 nm. Repeatability relative standard deviations (RSDr) ranged from 0.64-3.0% for EP and 2.0-6.6% for PS, excluding the high protein drink mix. Reproducibility relative standard deviations (RSDR) ranged from 2.1-6.6% for EP and 9.0-11.4% for PS, excluding the high protein drink mix. Recoveries ranged from 84.7-87.2% for EP and 84.6-98.2% for PS. The data developed for the minor alkaloids are more variable with generally unsatisfactory HORRATS (i.e., >2). However, since these alkaloids generally add little to the total alkaloid content of the products, the method gives satisfactory results in measuring total alkaloid content (RSDr 0.85-3.13%; RSDR 2.03-10.97%, HORRAT 0.69-3.23, exclusive of the results from the high protein drink). On the basis of these results, the method is recommended for Official First Action for determination of EP and PS in dietary supplements exclusive of the high protein drinks. 相似文献
52.
The modified ionic and covalent valence indices are introduced, defined in the framework of the two-particle density matrix, with respect to the reference state of separated atoms or ions (SAL ). They include only quadratic contributions in changes of the molecular charge-and-bond order matrix elements, relative to the SAL . General properties of the modified valence indices are examined and illustrative qualitative results for model systems are presented. Numerical UHF SCF MO valence data for selected diatomic and triatomic molecules are reported and interpreted in terms of the valence saturation effect and the ionic vs. covalent valence competition. A three-orbital valence model of a symmetric transition state of the bond-forming–bond-breaking reaction supports the BEBO model postulate of preservation of the total “bond order.” The model predictions are compared with the UHF numerical values. © 1994 John Wiley & Sons, Inc. 相似文献
53.
[formula: see text] The reaction of secondary and primary alcohols with highly fluorinated 3,4,5-tris(5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,12-heptadecafluorododecan- 1-yloxy)benzoic acid in the presence of Ph3P and DIAD in THF at room temperature (fluorous Mitsunobu) resulted in a simple, chromatography-free isolation protocol with excellent yields (83-96%). 相似文献
54.
Piotr Kutrowski Dominika Sukowska Renata Pytlowany Roman Dziembaj 《Reaction Kinetics and Catalysis Letters》2004,81(1):3-11
Catalytic performance of Ba(OH)2 and Sr(OH)2 in self-condensation of acetone was examined in the temperature range from 273 to 303 K. A kinetic model of second order with respect to acetone was used for interpretation of the results obtained for the diacetone alcohol formation.This revised version was published online in December 2005 with corrections to the Cover Date. 相似文献
55.
The40Ar/39Ar technique is an analytical variation of the K–Ar dating method. A known fraction of the39K in a sample is converted to39Ar by irradiation with fast neutrons. In an incremental heating experiment, the argon is released from the sample fractionally by stepwise heating. The result is a series of apparent ages.40Ar/39Ar age spectrum was determined for the sample Oase Vestfold. The minimum of the saddle-shaped age spectrum gives 1.0 billion years. 相似文献
56.
57.
S. Jakobs Ulrike Schulz Angela Duparré Norbert Kaiser 《Analytical and bioanalytical chemistry》1997,358(1-2):242-244
SiO2 protective coatings have been deposited on polycarbonate substrates by plasma ion assisted deposition. The influence of ion energy on the water permeability and the surface topography of the coatings was studied by infrared spectroscopy and atomic force microscopy. Coatings deposited at sufficiently high ion energies show a barrier effect against moisture uptake and considerably reduced film roughness. Both effects are attributed to an increase of the packing densities of the coatings. 相似文献
58.
Roman Luboradzki Janusz Lipkowski Yurii A. Simonov Marina S. Fonari Edward V. Ganin Arkadii A. Yavolovskii 《Journal of inclusion phenomena and macrocyclic chemistry》1995,23(3):181-193
An X-ray—diffraction study is reported for two molecular complexes containing 3,4-diamino-1,2,5-oxadiazole as guest (G) with 18-crown-6 (18-C-6) andcis-anti-cis-dicyclohexano-18-crown-6 (DCH-6B) as host. Both complexes are of the polymeric-chain structure with the guest molecule bridging two crown neighbours. ComplexI: [18-C-6*G*H2O], 111, monoclinic,P21/n,a=8.171(1),b=15.042(2),c=16.209(6) Å, =101.15(2)°, finalR-factor 0.068. ComplexII: [DCH-6B*G], 11, monoclinicC2/c,a=21.212(4),b=9.380(2),c=13.049(3) Å, =108.61(3)°, finalR 0.047. 相似文献
59.
Roman B?aszczyk 《Tetrahedron letters》2007,48(33):5859-5863
An efficient, diastereoselective synthesis of 5-substituted (2-thioxo-imidazolidin-4-yl)phosphonic acid diethyl esters from metallated diethyl isothiocyanatomethylphosphonate and activated imines has been developed. The three-step transformation of imidazolidine-2-thione derivatives into 1,2-diaminoalkylphosphonic acids is also described. 相似文献
60.
Tomcík P Jencusová P Krajcíková M Bustin D Brescher R 《Analytical and bioanalytical chemistry》2005,383(5):864-868
An interdigitated microelectrode array (IDA) was applied to the determination of formaldehyde released from textiles produced
in industry. The proposed method is based on formaldehyde reaction with hypobromite which is formed in weakly basic media
by control current electrooxidation of bromide on the generator segment of the IDA array. The unreacted hypobromite diffuses
through the gap between individually polarisable IDA segments and it is amperometrically detected on the collector segment
of the IDA. The efficiency of this nonconvective transfer process in the absence of formaldehyde was substantially higher
(78%) in comparison with that when using the rotating ring disc electrode. The influence of the added formaldehyde on the
transfer process can be utilised to develop a simple and sensitive analytical procedure for formaldehyde detection with a
detection limit of 4×10−6 mol dm−3. 相似文献