Direct analysis of thin-layer chromatographic spots of narcotics by means of diffuse reflectance Fourier transform infrared spectroscopy

The technique of diffuse reflectance Fourier transform infrared spectrometry (DRIFT) as an in situ detection method was used for the qualitative and quantitative analysis of drugs (heroin, cocaine and codeine) separated by thin layer chromatography.It was found that at a given interferometer throughput and detector sensitivity the quality of the spectrum depends strongly in the type of the chromatographic thin layer used. A detection limit of approx. 2 g was attained on a microcrystalline cellulose thin layer with a dynamically aligned Bio-Rad Digilab FTS 60A/896 type interferometer and room temperature DTGS detector. A reliable qualitative analysis can be made with as little as 10 to 15 g drug per spot.     

Lyotropic effect in surface charge,electrokinetics, and coagulation of a rutile dispersion

Potentiometric, electrokinetic, and coagulation experiments with a rutile dispersion in the pH region above the point of zero charge exhibit an inverse lyotropic sequence for counterions: Li⁺>K⁺>Cs⁺. The potentiometric and electrokinetic data were interpreted by a surface complexation model assuming the Stern-Gouy-Chapman structure of the interfacial layer, which yielded the values of inner layer capacitances,C, and the intrinsic equilibrium constants,K _ass ⁰ , characterizing the specificity of each counterion. These parameters were used to explain the order of lyotropic sequences in the adsorption, coagulation, and electrokinetic phenomena.     

Characterization of the organization in shear layers via the Proper Orthogonal Decomposition

Experiments are performed in an incompressible plane turbulent mixing layer, using various hot wire rake configurations. From these experiments, the Proper Orthogonal Decomposition is applied for kernels where the space-time correlation tensor is evaluated over different spatial meshes and velocity components configurations. The resulting decompositions are then discussed in terms of characterization of the organization of the flow for various scalar or vectorial approaches of the POD. An incrtial range law is evidenced. The instantaneous contribution of the first modes of the POD to the organization of the flow is analyzed. A dynamical behavior for the organization of the flow is observed from the correlation between the first two modes contribution.     

HPLC study of the binding of sulfinpyrazone to serum albumin

Summary A thin layer chromatographic method for a qualitative screening-test and a quantitative analysis of 2,4,6-TNT, biodegradation products, octogen and hexogen in ammunition wastes was developed using both polar and non-polar modified sorbents. For enrichment a solidphase extraction on LiChrolut® EN followed by removal with methanol/acetonitrile (11 v/v) was chosen. To imitate real samples, spiked tap water samples of known composition were used.     

Identification of formylglycine in sulfatases by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

C(alpha)-Formylglycine, the catalytic amino acid residue in the active site of sulfatases, is generated by post-translational modification of a cysteine or serine residue. We describe a highly sensitive procedure for the detection of C(alpha)-formylglycine-containing peptides in tryptic digests of sulfatase proteins. The protocol is based on the formation of hydrazone derivatives of C(alpha)-formylglycine-containing peptides when using dinitrophenylhydrazine as a matrix for matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS). The hydrazone derivatives desorb and ionize with high efficiency and can be detected in the sub-femtomole range. The presence of C(alpha)-formylglycine is indicated by a mass increment of 180.13 u, corresponding to the hydrazone moiety, and also by a unique C-terminal fragment ion, characteristic of sulfatases, that becomes prominent in MALDI post-source decay mass spectra of the hydrazone derivatives.     

Flow injection manifolds for liquid-liquid extraction without phase separation assisted by ultrasound

Flow injection (FI) manifolds based on iterative change of the flow direction have been designed to study the influence of auxiliary energy on continuous liquid-liquid extraction without phase separation and compare it with the non-assisted process in a single experiment. In order to demonstrate the utility of ultrasounds as auxiliary energy for the extraction of polyphenols from an organic phase, the approach has been applied to samples of extra virgin olive oil, using an alkaline aqueous phase as extractant and subsequent derivatization with the Folin-Ciocalteu reagent. The proposed method provides results similar to those from the official method-recoveries between 97 and 100%. The sensitivity of the proposed method is 3.5 times higher than that of the non-ultrasound-assisted method. The precision, expressed as relative standard deviation (R.S.D.) for n=5, was within 1-5% and the relative errors for the irradiated and non-irradiated method were within 3 and 5%, respectively. The repeatability and within-laboratory reproducibility, studied at two concentration levels (379 and 813 μg ml⁻¹) ranged between 0.7-4.4% and 0.6-4.8%, respectively. The proposed manifolds can also be applied to either other type of auxiliary energies—microwave, thermal—or two different types of auxiliary energies at the same time.     

白藜芦醇分子的转动惯量和电偶极矩

通过分子轨道理论和杂化轨道理论推断出较稳定的白藜芦醇分子是平面型分子,然后根据白藜芦醇分子结构特点计算了该化合物的一种稳定异构体的转动惯量,用矢量合成法计算了其电偶极矩,为微波辅助白藜芦醇萃取理论研究提供转动惯量和电偶极矩的数据.     

Dynamic ultrasound-assisted extraction of polyphenols in tobacco

A novel extraction method, namely dynamic ultrasound-assisted extraction, is investigated. This technique is efficient with respect to both time and solvent consumption because it utilizes ultrasonic energy in dynamic mode during extraction. Polyphenols (chlorogenic acid, esculetin, rutin, scopoletin, and quercitrin) are extracted from a tobacco (Nicotina tobaccum L.) sample for 10 min with 6 mL of solvent. Fresh solvent is continuously pumped through the sample, with which the analytes can be rapidly extracted, and the possibility of degradation efficiently avoided. Methanol involving 0.5% w/v ascorbic acid was used as extraction solvent; optimal flow rate and extraction time were investigated. The extract was cleaned up by C18 disposable cartridge. The spiked and nonspiked tobacco samples were used for the evaluation of the proposed method. Recoveries obtained were varied from 96 to 108% and RSDs from 2.0 to 4.6%. This extraction technique was revealed to recover larger amounts of polyphenols from tobacco, compared to the static ultrasound-assisted extraction method.     

Structure–retardation factor relationship of natural amino acids in two different mobile phases of RP-TLC

Abstract

Separation of amino acids (AAs) and their simple and inexpensive determination/identification is an interesting topic in biological and protein science, different food industries, and drug factories. Also, the presentation of the chromatographic behavior of compounds in a predictive model can be effective to estimate the structural/chemical properties of analyte and mobile phases. In this work for the first time, retardation factor (R_F) of 42 AAs in reversed-phase thin layer chromatography (RP-TLC) was modeled. Acetonitrile-sodium azide solution and 1,2 dioxane-sodium azide solution were two mobile phases which have been studied in this work. Results showed that the values of R_F are correlated with the structural properties of AAs and these properties had some similarities and differences in two noted mobile phases. For the TLC data in two mobile phases, five parametric linear models were suggested (R²_train = 0.93 and 0.97; R²_test = 0.93 and 0.99). The models were also evaluated with different statistical approaches. It was shown that increasing the sum of geometrical distances between N and O in AAs causes decreasing their R_F in RP-TLC using both mobile phases. Other structural effects of AAs on their separation in the desired RP-TLC system were also discussed.     

Thermal analysis and X-ray studies of chiral ferroelectric liquid crystalline materials and their binary mixtures

Summary Thermal properties of a homologous series of ferroelectric liquid crystals S-(-)-[4-(2-n-alkoxy-propionyloxy)]biphenyl-4'-[n-alkoxy-(3,5-dimethyl)]benzoate have been investigated by polarizing optical microscopy and differential scanning calorimetry. The mesophases were identified and confirmed by X-ray too. Three binary mixtures were prepared from the individual homologues. In one of the mixtures (Mix1), the ferroelectric SmC* phase has broadened and became enantiotropic. This mesophase remained monotropic in the other two mixtures (Mix2, Mix3). The chiral nematic N* phase did not appear in Mix1, but remained monotropic for the other two mixtures. Two molecular parameters, the layer spacing and the average intermolecular distance have been calculated from the X-ray results for the homologues and their mixtures. An intercalated tail-to-tail packing of molecules was found both in the single compounds and their mixtures resulting in the layer spacing about half of the molecular length of the single compounds.