Separation and identification of a new saponin from the flowers of Guaiacum officinale L

A triterpenoid saponin, guaianin O (1), oleanolic acid 3-O-{α-L-rhamnopyranosyl-(1 → 2)-[β-D-glucopyranosyl-(1 → 3)]-α-L-arabinopyranoside}-28- O-[β-D-glucopyranosyl]-ester, was isolated from the n-butanol extract of flowers of Guaiacum officinale L. The structural elucidation of 1 was accomplished by extensive studies of both one and two dimensional 1H, 13C-NMR spectra, the FAB mass spectrum, and alkaline and acid hydrolyses.     

A simple and rapid dispersive liquid-liquid microextraction method followed by GC-FID for determination of N-methylpyrrolidine in cefepime

A simple, rapid and efficient sample preparation technique, dispersive liquid-liquid microextraction, coupled with gas chromatography-flame ionization detection has been developed to determine N-methylpyrrolidine in cefepime. The effect of various experimental factors on the preparation procedure, such as the nature and volume of extraction and disperser solvents, extraction time, the nature of buffer and its pH, and salt effect, was investigated, optimized and the following results were obtained: extraction solvent, chloroform; dispersive solvent and solvent for dissolving cefepime, a mixture of methanol/water (88:12, v/v); salting out agent, NaCl; and buffer, carbonate/bicarbonate (C=0.5?M, pH=12). The optimized conditions were applied to the real sample (cefepime) for the extraction and determination of N-methylpyrrolidine. The calibration graph is linear from 0.02 to 850?mg/L with the square of correlation coefficient 0.999. LOD and LOQ are 6.4 and 21.2?μg/L in solution, respectively, and 0.2 (2×10(-5) ) and 0.6 (6×10(-5) ) μg/g (%, w/w) in cefepime powder, respectively, using sample size 50?mg. Repeatability of the method is good and RSD% for six repeated experiments (C=170?mg/L) is 6.35%.     

Optimized ultrasound‐assisted extraction procedure for the analysis of opium alkaloids in papaver plants by cyclodextrin‐modified capillary electrophoresis

This study investigated the use of ultrasound‐assisted extraction to improve the extraction efficiency of morphine, codeine and thebaine from the papaver plants. Extraction conditions such as type of solvent, temperature, duration, frequency and power level of ultrasonic were optimized and the influences of different parameters on resolution of alkaloids in CE were studied. The optimized condition for CE separation includes a sodium phosphate buffer (100 mM, pH 3.0) containing 5 mM α‐CD. The optimized extraction conditions for ultrasound‐assisted extraction was an extraction time of 1 h, an ultrasonic frequency of 60 kHz with water–methanol (80:20) at 40°C as the extraction solvent. The LOD for alkaloids was found to be 0.1 μg/mL at a signal‐to‐noise ratio of 3:1. The RSDs for peak areas were in the range of 1.4–4.4%. The amounts of opium alkaloids (mg/100 g dried sample) in four Iranian papaver plants were found to be in the range of 7.8–8.7 (morphine), 5.5–9.5 (codeine) and 1.4–10.4 (thebaine). It should be emphasized that no cleanup of the filtered extract was required; hence, direct determination after extraction drastically simplifies the analytical process.     

Étude structurale de britholite au césium Sr7La2Cs(PO4)5(SiO4)F2

Several studies demonstrated the ability of britholites to retain radionuclides such as the caesium and actinides. Therefore, three compounds with formulas Sr₈LaCs(PO₄)₆F₂, Sr₇La₂Cs(PO₄)₅(SiO₄)F₂ and Sr₂La₇Cs(SiO₄)₆F₂, were prepared by solid state reaction. However, it seems that only the mono-silicated composition was obtained in a pure state. In this present work, the X-ray diffraction and magnetic nuclear resonance have been used to investigate the structure for this composition. The results showed that in fact this phase was not pure, but it was mixed with a secondary phase, SrLaCs(PO₄)₂. The refinement by the Rietveld method allowed also to precise the distribution of La³⁺ and Cs⁺ ions between the two cationic sites of the apatite.     

Quantitative determination of chemical constituents from seeds of Nigella sativa L. using HPLC-UV and identification by LC-ESI-TOF

An HPLC method was developed for the simultaneous determination of nine compounds of Nigella sativa L. The separation was achieved within 23 min by using C18 column material, a water-acetonitrile mobile phase, both containing 0.1% acetic acid gradient system and a temperature of 35 degrees C. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ of nine compounds were in the range of 0.09-10 and 0.3-25 microg/mL, respectively. The wavelength used for quantification with the diode array detector was 205 and 260 nm. LC/MS coupled with electrospray ionization interface method is described for the identification of compounds in N. sativa L. samples. This method involved the use of [M+H]+ and [M+Na]+ ions in the positive ion mode with extracted ion chromatogram.     

In vitro antitumor and antibacterial assay of organotin(IV) complexes of 2,3-methylenedioxybenzoic acid; X-ray crystal structure of [(C2H5)2Sn(C8H5O4)2]

New organotin(IV) compounds containing the carboxylate ligand 2,3-methylenedioxybenzoic acid (HL) have been synthesized with the general formula R₂SnL₂ (R = Me, Et, n-Bu, Ph and n-Oct) and R₃SnL (R = n-Bu). All compounds have been studied in the solution state by multinuclear NMR (¹H, ¹³C and ¹¹⁹Sn) by using the non-coordinating solvent and also in solid sate by FTIR, mass spectrometry and X-ray crystallography. Spectroscopic data have shown that methylenedioxy moiety does not coordinate with tin atom and the coordination site is actually -COO group, as is proved by X-ray structure determination. The solid state structure of compound (2) has been determined by X-ray crystallography which shows that the complex (2) has distorted octahedral geometry. These complexes have been evaluated in vitro against crown gall tumor and antibacterial activity. Interesting results were noticed during the bio-activity screenings, which proved their in vitro biological potential and possible use as drugs.     

Thermokinetic studies of organotin(IV) carboxylates derived from para-methoxyphenylethanoic acid

Thremogravimetric (TG) studies of a new series of organotin(IV) carboxylates of the general formula R_nSnL_4-n (where R = CH₃, C₂H₅, C₄H₉, C₆H₅, C₆H₁₁ and C₈H₁₇, n = 2, 3 and L = para-methoxyphenylethanoate anion) have been carried out. Horowitz and Metzger method has been used to calculate thermokinetic parameters. It has been found that diorganotin dicarboxylates have larger activation energy than those of corresponding triorganotin carboxylates. Furthermore, the activation energy, Gibb’s free energy, entropy and enthalpy of diorganotin compounds shows the following trend, (CH₃)₂SnL₂ < (C₂H₅)₂SnL₂ < (C₄H₉)₂SnL₂ < (C₈H₁₇)₂SnL₂. This is attributed to steady increase in chain length of the alkyl groups. However, triorganotin compounds do not show such behavior.     

Similarities and Differences of the Active Sites in Basic and Advanced MgCl2‐Supported Ziegler‐Natta Propylene Polymerization Catalysts

Though preparation procedures of heterogeneous Ziegler‐Natta catalysts for propylene polymerization are sophisticated, it is uncertain whether the nature of the active sites is similar or different for different preparation procedures. In this study, the effects of preparation procedures on the nature of the active sites were investigated by stopped‐flow polymerization in combination with microstructure analysis of polymers. Both basic and advanced types of catalysts showed the same two kinds of isospecific active site, which indicated little influence of the preparation method on the active site structure. On the contrary, the ratios of the two kinds of isospecific sites were not the same, resulting in variation of average polymer properties.

     

Simultaneous microemulsion liquid chromatographic analysis of fat-soluble vitamins in pharmaceutical formulations: Optimization using genetic algorithm

An environmentally benign and simple method has been proposed for separation and determination of fat-soluble vitamins using isocratic microemulsion liquid chromatography. Optimization of parameters affecting the separation selectivity and efficiency including surfactant concentration, percent of cosurfactant (1-butanol), and percent of organic oily solvent (diethyl ether), temperature and pH were performed simultaneously using genetic algorithm method. A new software package, MLR-GA, was developed for this purpose. The results indicated that 73.6 mM sodium dodecyl sulfate, 13.64% (v/v) 1-butanol, 0.48% (v/v) diethyl ether, column temperature of 32.5 °C and 0.02 M phosphate buffer of pH 6.99 are the best conditions for separation of fat-soluble vitamins. At the optimized conditions, the calibration plots for the vitamins were obtained and detection limits (1.06–3.69 μg mL⁻¹), accuracy (recoveries > 94.3), precision (RSD < 3.96) and linearity (0.01–10 mg mL⁻¹) were estimated. Finally, the amount of vitamins in multivitamin syrup and a sample of fish oil capsule were determined. The results showed a good agreement with those reported by manufactures.