JSCS Vol 75, No. 7
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J. Serb. Chem. Soc. 75 (7) 875–891 (2010)
UDC
582.951.4.002.68+547.56+543:577.164.3; JSCS–4014; doi: 10.2298/JSC091109055W; Original scientific paper
Discrimination and classification of
tobacco wastes by identification and quantification of polyphenols with
LC–MS/MS
JUN WANG*,**, DINGQIANG LU*, HUI ZHAO*, BEN JIANG*, JIALI WANG*,
XIUQUAN LING*, HONG CHAI* and PINGKAI OUYANG*
*School of Biotechnology and Pharmaceutical
Engineering, Nanjing University of Technology, Nanjing 210009, P. R. China
**School of Biotechnology and Environmental
Engineering, Jiangsu University of Science and Technology, Zhenjiang 212018, P.
R. China
(Received 9 November 2009, revised 25 February 2010)
The chemical composition of polyphenols in tobacco
waste was identified by HPLC-PDA–ESI/MS/MS and the contents of chlorogenic
acids and rutin in 10 varieties of tobacco wastes were determined by HPLC–UV.
The relationships between the contents of active polyphenols and the varieties
of tobacco wastes were interpreted by hierarchical cluster analysis (HCA) and
principal component analysis (PCA). The results showed that 15 polyphenols were
identified in a methanolic extract of dried tobacco waste. The tobacco wastes
were characterized by high levels of chlorogenic acids (3-CQA, 5-CQA, and
4-CQA) and rutin; their ranges in the 10 tobacco varieties were 0.116–0.196,
0.686–1.781, 0.094–0.192, and 0.413–0.998 %, respectively. According to
multivariate statistics models, two active compound variables can be considered
important for the discrimination of the varieties of tobacco wastes:
chlorogenic acids and rutin. Consequently, sAMples of 10 tobacco varieties were
characterized into three groups by HCA based on the PCA pattern. In conclusion,
tobacco waste could be used as a new pharmaceutical material for the production
of natural chlorogenic acids and rutin in the ethnopharmacological industry.
Keywords: tobacco (Nicotiana
tabacum L.) waste; HPLC–PDA–ESI/MS/MS; chlorogenic acids; rutin;
multivariate statistical analysis.
Full
Article - PDF 543 KB Available OnLine: 11. 05. 2010.
J. Serb. Chem. Soc. 75 (7)
893–902 (2010)
UDC 633.888:575.21:543.05(497.113);
JSCS–4015; doi: 10.2298/JSC091019070D; Original
scientific paper
Δ9-Tetrahydrocannabinol
content in cannabis sAMples seized in Novi Sad during 2008
MAJA DJURENDIĆ-BRENESEL, NIKŠA AJDUKOVIĆ, KATARINA
ŠTAJNIC-RISTIĆ, VLADIMIR PILIJA and IGOR VESELINOVIĆ
Institute of Forensic Medicine, Clinical Center
Vojvodina, Hajduk Veljkova 7–9, 21000 Novi Sad, Serbia
(Received 19 October, revised 15 December 2009)
The three main cannabinoids Δ9-tetrahydrocannabinol
(Δ9-THC), cannabidiol (CBD) and cannabinol (CBN) were identified and
determined quantitatively using a GCD (GC-EI) instrument in 280 sAMples of
illicit herbal cannabis, seized by the Police authorities in Novi Sad, during
2008. The sAMples were sent to the Institute of Forensic Medicine, Clinical
Center Vojvodina, for forensic chemical analysis. The cannabinoid content of
the sAMples enabled the classification of the cannabis into three chemical
phenotypes and the differentiation into drug and textile-cannabis, using the
Waller classification index. This differentiation has great forensic significance
in the classification of certain cases as a criminal action. The experimental
results showed that the Δ9-THC content in illicitly circulated
cannabis slightly decreased from January to December 2008, as did the quality
of the drug-cannabis. The reasons for the quality variations could lie in the
geographical origin of the cannabis plants, the conditions of plants storage,
various parts of the plants in sAMples and the time elapsed between harvesting
and chemical analysis.
Keywords:
cannabinoids; forensic sAMples; GCD
analysis; phenotype; Waller index.
Full
Article - PDF 339 KB Available OnLine: 12. 06. 2010.
J. Serb.
Chem. Soc. 75 (7) 903–915 (2010)
UDC 633.86+667.272/.276:543.544.5;
JSCS–4016; doi: 10.2298/JSC091027071G; Original
scientific paper
Determination of natural colorants in
plant extracts by high-performance liquid chromatography
RENETA GEVRENOVA
Department of Pharmacognosy, Faculty of
Pharmacy, Medical University – Sofia, Dunav str. 2, 1000 Sofia, Bulgaria
(Received 27 October 2009, revised 12
January 2010)
The
determination of the colouring compounds apigenin (1), lawsone (2), juglone
(3) and indigotin (4) in plant extracts using HPLC–UV/Vis
methods is reported. The methods were applied to the analysis of 1–4 in ethanolic and propylene glycolic
extracts originating, respectively, from chAMomile (ChAMomilla recutita [L] Rauschert, Asteraceae), henna (Lawsonia inermis L., Lythraceae), walnut
(Juglans regia L., Juglandaceae) and
natural indigo (Indigofera sp.,
Fabaceae). In the case of the indigo extracts, an optimized acid hydrolysis was
applied. HPLC separations were performed on a Hypersil ODS RP18 column using
linear gradient elution progrAMs. The detection limits for 1–4 were 0.11, 0.6, 0.10, 0.089 μg mL-1, respectively.
The procedure did not involve any sAMple “clean-up” methods. The AMounts of the
colouring compounds ranged from 0.006 (3) to 0.13 mg mL-1 (4) in the ethanolic extracts and from
0.22 (2) to 1.44 mg mL-1
(4) in propylene glycolic extracts.
The proposed HPLC methods are advantageous in terms of sAMple preparation and
the selective separation of the compounds. The plant dye extracts are commonly
used in hair colouring formulations. The results indicate that the methods
developed may serve for the quantitative control of dying plants and cosmetic
products.
Keywords:
apigenin; indigotin; juglone; lawsone; high-performance liquid chromatography.
Full Article - PDF 223 KB Available OnLine: 12. 06. 2010.
J. Serb. Chem. Soc. 75 (7) 917–927 (2010)
UDC
547.1’128+547.79:542.9+547.571+547.551:615.281/.282; JSCS–4017; doi:
10.2298/JSC081216063S;
Original scientific paper
Synthetic, structural and biological
studies of organosilicon(IV) complexes of Schiff bases derived from
pyrrole-2-carboxaldehyde
KIRAN SINGH and DHARAM PAL*
Department of Chemistry, Kurukshetra University,
Kurukshetra-136 119, India
*Department of Applied Sciences, J.I.E.T.,
Jind-126102, Haryana, India
(Received 16 December 2008, revised 26 April 2010)
Selected new organosilicon(IV) complexes having the
general formula R2SiCl[L] and R2Si[L] 2 were
synthesized by the reactions of Me2SiCl2 with Schiff
bases (5-mercapto-4-[(1H-pyrrol-2ylmethylene)AMino]-s-triazole, 5-mercapto-3-methyl-4-[(1H-pyrrol-2ylmethylene)AMino]-s-triazole and 3-ethyl-5-mercapto-4-[(1H-pyrrol-2ylmethylene)AMino]-s-triazole) in 1:1 and 1:2 molar ratios.
All of the compounds were characterized by elemental analysis, molar
conductance, and IR, UV, 1H-, 13C- and 29Si-NMR
spectral studies. All the spectral data suggest an involvement with an
azomethine nitrogen in coordination to the central silicon atom. With the help
of above-mentioned spectral studies, penta and hexacoordinated environments
around the central silicon atoms in the 1:1 and 1:2 complexes, respectively,
are proposed. Finally, the free ligands and their metal complexes were tested in vitro against some pathogenic
bacteria and fungi to assess their antimicrobial properties.
Keywords: antifungal; antibacterial; silicon complexes;
s-triazole; Schiff bases.
Full Article - PDF 211 KB Available OnLine: 01. 06. 2010.
UDC
546.262.5+661.8+547.583.1:544.146.2:543.42; JSCS–4018; doi:
10.2298/JSC090825066K;
Original scientific paper
Preparation and characterization of novel oxo-centered basic p-chlorobenzoic bridging trinuclear
complexes
IMAN KHOSRAVI and MOHAMMAD YAZDANBAKHSH
Department of Chemistry, Faculty of Science, Ferdowsi University of
Mashhad, Mashhad, Iran
(Received 25 August 2009, revised 2 February 2010)
Three new oxo-centered trinuclear complexes, one of them a mixed-valence
complex [Mn3O(C7H4O2Cl)6(Py)3]Py
(1) and the others, mixed-metal
complexes of [Fe2MnO(C7H4O2Cl)6(Py)3]NO3
(2) and [Fe2CoO(C7H4O2Cl)6(Py)3]
(3) were synthesized by the direct
reaction between metal nitrates and p-chlorobenzoic
acid. These complexes were characterized by elemental analyses (CHN), atomic
absorption spectroscopy and spectral (IR, electronic) studies. These are new
type of oxo-bridged mixed-metal complexes in which the carboxylate ligand is p-chlorobenzoic acid. The UV spectra of
the complexes exhibited a strong band in the region 42,500 cm-1
which is related to the (π → π*) transitions of the pyridine ligand. The IR
spectra of these compounds showed two strong stretching vibrations bands,
indicating a bridging coordination mode of the carboxylic group of the ligand
in the complexes.
Keywords: mixed-valence; oxo-centered; trinuclear complexes;
spectroscopy; carboxylic ligand; IR spectra.
Full Article - PDF 164 KB Available OnLine: 01. 06. 2010.
J. Serb. Chem. Soc. 75 (7) 935–941 (2010)
UDC 546.732’742’562.004.12:547.455.4;
JSCS–4019; doi: 10.2298/JSC090804069C;
Original scientific paper
Synthesis and characterization of a tetraaza macrocyclic ligand and its
cobalt(II), nickel(II) and copper(II) complexes
SULEKH CHANDRA, MONIKA TYAGI and SWATI AGARWAL*
Department of Chemistry, Zakir Husain College
(University of Delhi), JLN-Marg, New Delhi – 110002, India
*Department of Chemistry, Motilal Nehru College
(University of Delhi), Benito Juarez Road, New Delhi – 110 021, India
(Received 18 September, revised 7 December 2009)
Co(II), Ni(II), and Cu(II) complexes with a
tetradentate nitrogen donor [N4] macrocyclic ligand, viz. 6,15-dimethyl-8,17diphenyl-7,16-dihydrodibenzo[b,i][1.4.8.11]tetraazacyclotetradecine,
were synthesized. Their structures were determined based on elemental analyses,
molar conductance and magnetic susceptibility measurements, and IR, 1H-NMR
(ligand) and electronic spectral studies. Based on analytical and molar
conductance data, the complexes may be formulated as [M(L)Cl2] and
[M’(L)]Cl2 (where M = Co(II) and Cu(II), and M’ = Ni(II)) due to
their non-electrolytic and 1:2 electrolytic nature. Based on spectral studies,
an octahedral geometry was assigned for the Co(II) complex, whereas
square-planar and tetragonal geometry were proposed for the Ni(II) and Cu(II)
complexes, respectively. The synthesized ligand and its complexes were screened
for fungicidal activity against two pathogenic fungi (i.e., Fusarium moniliformae and
Rhizoctonia solani) to assess their
growth inhibiting potential.
Keywords: tetraaza macrocycle;
Co(II), Ni(II) and Cu(II) complexes; characterization.
Full
Article - PDF 200 KB Available OnLine: 12. 06. 2010.
J. Serb. Chem. Soc. 75 (7) 943–950 (2010)
UDC 547.538.2+66.095.252:537.872:539.193; JSCS–4020; doi: 10.2298/JSC091201068J; Original
scientific paper
Cyclic conjugation in benzo-annelated
triphenylenes
SVETLANA
JEREMIĆ, SLAVKO RADENKOVIĆ and IVAN GUTMAN
Faculty of
Science, University of Kragujevac, P. O. Box 60, 34000 Kragujevac, Serbia
(Received 1
December 2009)
Cyclic conjugation in benzo-annelated
triphenylenes was studied by means of the energy effect (ef) and the π-electron
content (EC) of the six-membered rings. A regularity that was earlier
discovered in the case of acenaphthylene and fluoranthene congeners is now
shown to hold also for benzo-annelated triphenylenes: Benzenoid rings that are
annelated angularly with regard to the central six-membered ring Z0
of triphenylene increase the intensity of the cyclic conjugation in Z0,
whereas linearly annelated benzenoid rings decrease the cyclic conjugation in Z0.
The ef- and EC-values are strongly correlated, yet in a non-linear
manner.
Keywords: cyclic conjugation; energy effect of cyclic conjugation; triphenylene;
benzo-annelated triphenylene.
Full Article - PDF 280 KB Available OnLine: 03. 06. 2010.
J. Serb. Chem. Soc. 75 (7) 951–963 (2010)
UDC 546.39’185+546.27+542.913; JSCS–4021; doi:
10.2298/JSC090228064M; Original scientific paper
Synthesis and
characterization of AMmonium phosphate fertilizers with boron
ANGELA MAGDA, RODICA PODE,
CORNELIA MUNTEAN, MIHAI MEDELEANU and ALEXANDRU POPA*
Faculty of Industrial
Chemistry and Environmental Engineering, “Politehnica” University of Timişoara,
Victoria Square 2, 300006 Timişoara, Romania
*Institute of Chemistry
Timisoara of the Romanian Academy, M. Viteazul Ave, 24, 300223-Timisoara,
Romania
(Received 28 February 2009,
revised 26 April 2010)
The concentration of boron,
an essential micronutrient for plants, presents a narrow range between
deficiency and toxicity. In order to provide the boron requirement for plants,
and to avoid toxicity problems, boron compounds are mixed with basic
fertilizers. Sodium borate pentahydrate was used as a boron source. Ammonium
orthophosphates fertilizers with boron were prepared by neutralizing phosphoric
acid with AMmonia and addition of variable AMounts of sodium tetraborate
pentahydrate to the reaction mixture at a NH3:H3PO4
molar ratio of 1.5. The fertilizers obtained with boron contents ranging from
0.05 to 1 % (w/w) were fully characterized by chemical analysis, thermal
analysis, X-ray diffraction and infrared spectrophotometry. The studies showed
that up to 500 °C, regardless of the boron content, no significant changes
concerning thermal stability and nutritional properties occurred. Above 500 °C,
an increase of thermal stability with an increase of the boron content was
observed. X-Ray diffraction of a heat-treated sAMple containing 5 % (w/w) boron
indicated the appearance of boron orthophosphate, BPO4, as a new
crystalline phase, and the disappearance of the previous structures above 500
°C, which explains the increase in thermal stability.
Keywords: sodium borate pentahydrate; fertilizer;
micronutrient; diAMmonium hydrogen phosphate; AMmonium dihydrogen phosphate;
boron orthophosphate.
Full Article - PDF 312 KB Available OnLine: 01. 06. 2010.
J. Serb. Chem. Soc. 75 (7)
965–973 (2010)
UDC
666.32+661.182+66.094.3:61.000.57; JSCS–4022, doi: 10.2298/JSC090617062J; Original
scientific paper
Singlet oxygen generation
by higher fullerene-based colloids
SVETLANA P. JOVANOVIĆ, ZORAN M. MARKOVIĆ,
DUŠKA N. KLEUT, VLADIMIR D. TRAJKOVIĆ*, BRANKA S. BABIĆ-STOJIĆ, MIROSLAV D.
DRAMIĆANIN and BILJANA M. TODOROVIĆ MARKOVIĆ
Vinča Institute, P.O. Box 522, 11001
Belgrade, Serbia
*Institute of Microbiology and Immunology,
School of Medicine, University of Belgrade, Dr. Subotića 1, 11000 Belgrade,
Serbia
(Received 17 June 2009, revised 26 April
2010)
In this paper, the results
of the synthesis and characterization of higher fullerene-based colloids is
presented. The generation of singlet oxygen 1O2 (1Δg) by fullerene
water-based colloids (nC60, nC70 and nC84) was
investigated. It was found by electron parAMagnetic resonance spectroscopy that
the generation of singlet oxygen was the highest by the nC84 colloid.
The AMplitude of the electron parAMagnetic resonance (EPR) signal was two
orders of magnitude higher than the AMplitude of the EPR signals which
originated from nC60 and nC70. The surface morphology and the
structure of the particles of the water-based colloids were investigated by
atomic force microscopy (AFM). The AFM study showed that the average size of
the nC60, nC70 and nC84 were 200, 80 and 70 nm,
respectively. In addition, the particle size distribution of the nC60, nC70
and nC84 colloids was determined by dynAMic light scattering (DLS)
measurements.
Keywords: higher fullerene; colloid; electron parAMagnetic
resonance spectroscopy; atomic force microscopy; dynAMic light scattering.
Full Article - PDF 321 KB Available OnLine: 28. 05. 2010.
J. Serb. Chem. Soc. 75 (7) 975–985 (2010)
UDC
615.453.4+546.131:543.544.5.068.7; JSCS–4023; doi:
10.2298/JSC090728065M; Original scientific paper
Development and application
of a validated HPLC method for the analysis of dissolution sAMples of
mexiletine hydrochloride capsules
DRAGAN M. MILENOVIĆ and
ZORAN B.TODOROVIĆ*
“Zdravlje-Actavis” Company,
Analytical Department, R &AMp; D, Vlajkova 199, 16000 Leskovac, Serbia
*Faculty of Technology,
Bulevar oslobođenja 124, 16000 Leskovac, University of Niš, Serbia
(Received 28 July 2009,
revised 16 February 2010)
The aim of this work was to
develop and validate a simple, efficient, sensitive and selective method for
the analysis of dissolution sAMples of mexiletine hydrochloride capsules by
HPLC without the necessity of any time-consuming extraction, dilution or
evaporation steps prior to drug assay. Separation was performed isocratically
on a 5 µm LiChrospher 60, RP-Select B column (250·4 mm ID) using the mobile
phase buffer–acetonitrile (60:42, v/v) at a flow rate of 1.2 mL min-1
and UV detection at 262 nm. The elution occurred in less than 10 min. The assay
was linear in the concentration range 50–300 µg mL-1 (r2
= 0.9998). The validation characteristics included accuracy, precision,
linearity, specificity, limits of detection and quantification, stability, and
robustness. Validation acceptance criteria were met in all cases (the percent
recoveries ranged between 100.01 and 101.68 %, RSD < 0.44 %). The
method could be used for the determination of mexiletine hydrochloride and for
monitoring its concentration in in vitro dissolution studies.
Keywords: mexiletine hydrochloride; dissolution; method
validation; HPLC.
Full Article - PDF 245 KB Available OnLine: 01. 06. 2010.
J. Serb. Chem. Soc. 75 (7)
987–996 (2010)
UDC
678.544:544.35:546.131+546.32–36; JSCS–4024; doi:
10.2298/JSC091009073L; Original scientific paper
A study on the
microstructure of a nitrate ester plasticized polyether propellant dissolved in
HCl and KOH solutions
YONG LIU*,**,
LUOXIN WANG***, XINLIN TUO**, SONGNIAN LI*,** and WEIMIN YANG*
*College of Mechanical and
Electrical Engineering, Beijing University of Chemical Technology, Beijing
100029, China
**Department of Chemical
Engineering, Tsinghua University, Beijing 100084, China
***Wuhan University of
Science and Engineering, Key Laboratory of Green Processing and Functional
Textiles of New Textile Materials, Ministry of Education, Wuhan 430073, China
(Received 9 October 2009,
revised 19 January 2010)
Understanding of how the
properties and performance of nitrate ester plasticized polyether (NEPE)
propellants relate to microstructure is complicated by numerous components that
have different characteristics. One approach to alleviating these complications
is to observe a microstructure that has lost one or several components. This
article exAMines the dissolution process, mass loss and change of the ion
concentration of propellants in acid and alkali solutions. A scanning electron
microscope was used to observe the dissolved residual of the propellants. The
results revealed that the main constituents of NEPE propellant have different
dissolving properties in solutions of HCl and KOH. By monitoring the
dissolution process of NEPE propellant in HCl and KOH solutions, it was found
that the microstructure of the propellant is generally compact and the polymer
binder not only binds all the other components, but also protects the inner
part of the propellant in solution.
Keywords: NEPE propellants; microstructure; interfaces;
scanning electron microscope (SEM); swelling.
Full Article - PDF 486 KB Available OnLine: 14. 06. 2010.
J. Serb. Chem. Soc. 75 (7)
997–1003 (2010)
UDC 547.21:536.423.1; JSCS–4025; doi:
10.2298/JSC091123067J; Note
NOTE
Reliable prediction of heat
of vaporization of n-alkanes at 298.15 K
JOVAN D. JOVANOVIĆ and
DUŠAN K. GROZDANIĆ
Faculty of Technology and
Metallurgy, University of Belgrade, Karnegijeva 4, 11000 Belgrade, Serbia
(Received 23 November 2009,
revised 3 March 2010)
A reliable model for the
prediction of the heat of vaporization for n-alkanes at 298.15 K with
the number of carbon atoms and normal boiling point as the only input
parAMeters is recommended. The new model is compared with other literature
models and was found to give the best results with absolute mean percentage
deviation of 0.81 % and maximum absolute percentage deviation of 2.93 %.
Keywords: heat of vaporization; n-alkanes;
prediction; model.
Full Article - PDF 168 KB Available OnLine: 03. 06. 2010.
J. Serb. Chem. Soc. 75 (7)
1005–1018 (2010)
UDC
504.45.055+549.25+556.16:504.06; JSCS–4026; doi:
10.2298/JSC090217061P; Original scientific paper
A simulation experiment as
a method for the investigation of the mobility of heavy metals from inundated
land
DJOKICA PETROVIĆ, MARIJA
TODOROVIĆ*, DRAGAN MANOJLOVIĆ* and VOJIN D. KRSMANOVIĆ*
Vinča Institute, Laboratory
for Radioisotopes, P.O. Box 522, 11001 Belgrade, Serbia
*Faculty of Chemistry,
University of Belgrade, P.O. Box 51, 11158 Belgrade 118, PAK: 105305, Serbia
(Received 17 February 2009,
revised 4 May 2010)
A simulation experiment was
used to study the interaction of river water with different soils (arable land,
orchards, meadows, pastures and forestland). The results obtained by sequential
extraction before and after the simulation experiment were compared in order to
determine the substrates of the heavy metals in inundated land and to evaluate
their mobility. SAMples of various soils were collected from the region of the
future accumulation Lake Bogovina (Serbia) and analysed for ten elements using
AAS, GFAAS and ICP. Investigation of the nature of the association of heavy
metals and the identification of their substrates were provided by a five-step
sequential extraction. Correlation analysis was used as a method for the
determination of the substrates for heavy metals. The good correlation AMong
the microelements and certain macroelements indicated the substrates of the
microelements. Manganese and iron had a good correlation with most of the
microelements. Calcium had only a few correlations with some microelements.
Some elements, such as nickel and cadmium, had one substrate before and another
after the simulation experiment.
Keywords: zinc; heavy metals; accumulation lake; sequential
extraction; inundated soil.
Full Article - PDF 393 KB Available OnLine: 28. 05. 2010.
Copyright
&AMp; copy; SHD 2010.
July 24, 2010.
For more information contact: JSCS-info@shd.org.rs