Simultaneous determination of noradrenaline and dopamine in Portulaca oleracea L. by capillary zone electrophoresis

A simple and rapid capillary electrophoretic method was developed for the simultaneous determination of noradrenaline (NA) and dopamine (DA) in Portulaca oleracea L. The buffer solution used in this method was 40 mM tris (hydroxymethyl) aminomethane (Tris)-H3PO4 at pH 2.00 containing 15% methanol. The effects of pH value, organic modifier, and applied voltage were investigated. The linear ranges of NA and DA were 0.5-100 microg/mL (r=0.9952) and 6.25-200 microg/mL (r=0.9992), respectively. The relative standard deviations of the corrected peak area were 6.73% and 4.26%, respectively. NA and DA in Portulaca oleracea L. were simultaneous determined successfully within 5.6 min. In this way, the contents of NA and DA in different parts (stem, leaves, and seeds) of P. oleracea L. and in different extracts of leaves with different solvents (distilled water, 50% methanol, and methanol) were studied.     

A new serratane-type triterpene from Lycopodium phlegmaria

A new serratane-type triterpene, lycophlegmarin (1), has been isolated from Lycopodium phlegmaria L. Four known related triterpenoids were also found from the title plant. The structure of the new compound was elucidated on the basis of detailed spectroscopic analysis and chemical method. Lycophlegmarin exhibited modest growth-inhibitory activity in vitro against human hepatoma cells BEL 7402.     

Baylis-Hillman reactions of N-tosyl aldimines and aryl aldehydes with 3-methylpenta-3,4-dien-2-one

The attempted Baylis-Hillman reactions of N-tosyl aldimines and aryl aldehydes with 3-methylpenta-3,4-dien-2-one gave the corresponding Baylis-Hillman adducts 3 and 6 in moderate to good yields in the presence of DMAP in DMSO, respectively. In the case of the aza-Baylis-Hillman reactions of N-tosyl aldimines with 3-methylpenta-3,4-dien-2-one catalyzed by PBu3, the corresponding aza-Baylis-Hillman derivatives 4 and 5 were formed at the same time.     

DOPING LEVEL INCREASE OF POLY(3-METHYLTHIOPHENE)FILM DURING ELECTROCHEMICAL POLYMERIZATION PROCESS

The Raman spectra of poly(3-methylthiophene) (PMeT) films with different thicknesses, which have beenelectrochemically deposited on a flat stainless steel electrode surface by direct oxidation of 3-methylthiophene in borontrifluoride diethyl etherate (BFEE) at a constant applied potential of 1.38 V (versus SCE), have been investigated byexcitation with a 633-nm laser beam. The spectroscopic results demonstrated that the doping level of PMeT film wasincreasing during film growth. This finding was also confirmed by electrochemical examination. Moreover, the Raman bandsassigned to radical cations and dications in doped PMeT films were found approximately at 1420 and 1400 cm~(-1),respectively. Radical cations and dications coexist on the backbone of PMeT as conductive species and their concentrationsincrease with the increase of doping level. Successive cyclic voltammetry was proved to be an effective approach toimproving the doping level of as-grown thin compact PMeT film.     

Optimization of the abnormal Beckmann rearrangement: application to steroid 17-oximes

A novel and practical procedure was developed for the abnormal Beckmann rearrangement of steroid 17-oximes. Treatment of the 17-oximes with TFA/CH(OMe)(3) in boiling THF for 2 h gives the corresponding 13,17-seco alkene nitrile products in unprecedented high yields (70-92%). Since the alkene nitriles can be subsequently converted into 18-norsteroids, this general method provides a highly efficient route to these biologically important compounds and, by extension, to other structurally related natural products.     

An HPLC and EPR investigation on the stability of DMPO and DMPO spin adducts in vivo

Application of the spin trapping technique in intact animals requires an understanding of the stability and distribution of the spin traps and their spin adducts in vivo. We studied the stability of DMPO in vivo in mice using HPLC and the stability of spin adducts of DMPO by EPR in plasma, whole blood, peritoneal fluid, and homogenized heart tissue of the rat. At 15 minutes after intraperitoneal injection DMPO had similar concentrations in the liver, heart, and blood of the mice and 40% remained in the organs 2 hours after the injection. In contrast, the spin adduct DMPO-OH was short lived, with a half-life of 3.0 minutes in plasma, and was not detectable 1 minute after formation in whole blood and homogenized heart tissue. The carbon centered spin adduct DMPO-CH(OH)CH₃ was more stable, having half-lives of 16, 11, 3.6, and 0.79 minutes in plasma, peritoneal fluid, whole blood, and homogenized heart tissue, respectively. The spin adduct DMPO-SO₃ was sufficiently stable for the adduct to be observed directly from living mice.     

Lattice disorder in silicon induced by 2.0 MeV Cu+ irradiation

The effect of 2.0 MeV Cu⁺ irradiation on Si(100) crystal has been studied by the Rutherford backscattering/channeling technique. Analysis of the lattice disorder distribution has been performed under 100 direction of tilting off from the target normal: 7°, 30°, and 45° as well as different doses. The lattice disorder distributions in Si(100) have been compared with TRIM'89 simulation. The results show that the lattice disorder distributions in Si(100) under different irradiation angles seem to be in good agreement with TRIM'89 simulation. When the dose increases up to 8.7×10¹⁴ ions/cm², the defect concentration increases leading to the formation of an amorphous layer.     

Luminescent heteronuclear Au(I)5Ag(I)8 complexes of [1,2,3-C6(C6H4R-4)3]3- (R = H, CH3, But) by cyclotrimerization of arylacetylides

Unusual AuI-AgI heterometallic complexes [Au5Ag8(mu-dppm)4{1,2,3-C6(C6H4R-4)3}(CCC6H4R-4)7]3+ (R = H 1, CH3 2, But 3) were isolated by reactions of polymeric silver arylacetylides (AgCCC6H4R-4)n with binuclear gold component [Au2(mu-dppm)2(MeCN)2]2+ (dppm = bis(diphenylphosphino)methane), in which cyclotrimerization of arylacetylide -CCC6H4R-4 affords trianion {1,2,3-C6(C6H4R-4)3}3- with an unprecedented mu5-bonding mode. Compounds 1(SbF6)3-3(SbF6)3 exhibit intense photoluminescence derived from an MLCT (Au5Ag8 --> CCC6H4R-4) transition, mixed with a metal cluster-centered excited states.