Determination of phenylephrine hydrochloride and chlorpheniramine maleate in binary mixture using chemometric-assisted spectrophotometric and high-performance liquid chromatographic-UV methods

Four methods have been developed for the simultaneous determination of phenylephrine hydrochloride and chlorpheniramine maleate without previous separation. In the first method both drugs are determined using first derivative UV spectrophotometry, with zero-crossing measurement. The second method depends on first derivative of the ratios spectra. The third method describes the use of multivariate spectrophotometric calibration for the simultaneous determination of the analyzed binary mixture where the resolution is accomplished by using partial least squares (PLS) regression analysis. In the fourth method (HPLC), a reversed-phase column and a mobile phase of methanol:water:acetonitrile (80:12:8 v/v/v/) at 0.9 ml/min flow rate have been used to separate both drugs with a UV detection at 270 nm. All the proposed methods are extensively validated. They have the advantage to be economic and time saving. All the described methods can be readily utilized for analysis of pharmaceutical formulations. The results obtained using the proposed methods are statistically analyzed and compared with some reported methods.     

Spectrophotometric Quantitation of Fluoxetine Hydrochloride Using Benzoyl Peroxide and Potassium Iodide

 Fluoxetine hydrochloride reacts with benzoyl peroxide and potassium iodide, after heating for 1 min at 30 °C, to give a blue colour having maximum absorbance at 570 nm. The reaction is selective for fluoxetine with 0.01 mg/mL as visual limit of quantitation and provides a basis for a new spectrophotometric determination. The colour reaction obeys Beer’s law from 0.1 mg/10 mL to 2.0 mg/10 mL of fluoxetine and the relative standard deviation is 0.68%. The qualitative assessment of tolerable amounts of other drugs is also studied. Received September 21, 1998. Revision September 10, 1999.     

Order of Reactivity of OH/NH Groups of Glucosamine Hydrochloride and N-Acetyl Glucosamine Toward Benzylation Using NaH/BnBr in DMF

The order of reactivity of OH and NH groups of glucosamine hydrochloride (GlcNH₂^.HCl) and N-acetyl glucosamine (GlcNAc) toward benzylation with NaH/BnBr in DMF was investigated. For GlcNH₂^.HCl, benzyl groups were introduced in the order of N-Bn > N-Bn₂ > 1-O-Bn > 6-O-Bn > 4-O-Bn > 3-O-Bn; for GlcNAc, benzyl groups were introduced in the order of 1-O-Bn > 6-O-Bn > 4-O-Bn > 3-O-Bn > N-Bn. A range of partially benzylated 2-N,N′-dibenzyl glucopyranosides and GlcNAc derivatives were obtained in a single step.     

新型胃动力药盐酸伊托必利的结构分析

本文以ＵＶ、ＦＴＩＲ、＾１Ｈ－ＮＭＲ、＾１３Ｃ－ＮＭＲ、ＦＡＢＭＳ等现代分析手段，对国内试制的新型胃动力药盐酸伊托必利的化学结构进行了分析鉴定。根据谱带与结构的对应关系，确证其结构与国外已报道的结构一致并对上述各种谱的谱带进行了全面的归属     

Sonocatalytic degradation of tetracycline hydrochloride with CoFe2O4/g-C3N4 composite

In this work, different mass percent ratios of CoFe₂O₄ coupled g-C₃N₄ (w%-CoFe₂O₄/g-C₃N₄, CFO/CN) nanocomposites were integrated through a hydrothermal process for the sonocatalytic eradication of tetracycline hydrochloride (TCH) from aqueous media. The prepared sonocatalysts were subjected to various techniques to investigate their morphology, crystallinity, ultrasound wave capturing activity and charge conductivity. From the investigated activity of the composite materials, it has been registered that the best sonocatalytic degradation efficiency of 26.71 % in 10 min was delivered when the amount of CoFe₂O₄ was 25% in the nanocomposite. The delivered efficiency was higher than that of bare CoFe₂O₄ and g-C₃N₄. This enriched sonocatalytic efficiency was credited to the accelerated charge transfer and separation of e⁻-h⁺ pair through the S-scheme heterojunctional interface. The trapping experiments confirmed that all the three species i.e. ^•OH, h⁺ and ^•O₂⁻ were involved in the eradication of antibiotics. A strong interaction was shown up between CoFe₂O₄ and g-C₃N₄ in the FTIR study to support charge transfer as confirmed from the photoluminescence and photocurrent analysis of the samples. This work will provide an easy approach for fabricating highly efficient low-cost magnetic sonocatalysts for the eradication of hazardous materials present in our environment.     

Inversion twinning in a second polymorph of the hydrochloride salt of the recreational drug ethylone

A second polymorph of the hydrochloride salt of the recreational drug ethylone, C₁₂H₁₆NO₃⁺·Cl⁻, is reported [systematic name: (±)‐2‐ethylammonio‐1‐(3,4‐methylenedioxyphenyl)propane‐1‐one chloride]. This polymorph, denoted form (A), appears in crystallizations performed above 308 K. The originally reported form (B) [Wood et al. (2015). Acta Cryst. C 71 , 32–38] crystallizes preferentially at room temperature. The conformations of the cations in the two forms differ by a 180° rotation about the C—C bond linking the side chain to the aromatic ring. Hydrogen bonding links the cations and anions in both forms into similar extended chains in which any one chain contains only a single enantiomer of the chiral cation, but the packing of the ions is different. In form (A), the aromatic rings of adjacent chains interleave, but pack equally well if neighbouring chains contain the same or opposite enantiomorph of the cation. The consequence of this is then near perfect inversion twinning in the structure. In form (B), neighbouring chains are always inverted, leading to a centrosymmetric space group. The question as to why the polymorphs crystallize at slightly different temperatures has been examined by density functional theory (DFT) and lattice energy calculations and a consideration of packing compactness. The free energy (ΔG) of the crystal lattice for polymorph (A) lies some 52 kJ mol⁻¹ above that of polymorph (B).     

Crystalline and spectroscopic characterization of poly(2-aminoethyl methacrylate hydrochloride) chains grafted onto poly[(R)-3-hydroxybutyric acid]

The present study is aimed to investigate the degree of crystallinity of poly(3-hydroxybutyrate) P(3HB) grafted with poly(2-aminoethyl methacrylate hydrochloride) (PAEMA) chains using WAXS, micro Raman, and FTIR spectroscopy. The samples were obtained by radiation induced graft polymerization of the monomer in the substrate using different solvents for comparison. The results of crystallinity are consistent with those obtained of lower crystallinity in grafting copolymer relative to the substrate P(3HB). The low crystallinity is directly related to the increase of the degree of grafting, meaning that although the P(3HB) amorphous region is grafted, the crystalline zone is also affected in some extent by the grafting process and the environment of the new molecule. Three different methods were surveyed to determine the variation of crystallinity degree with the grafting degree. It is shown that all methods provide linear relationships between these variables, but WAXS method was found more acceptable than the others (FTIR and Raman). A detailed characterization of the vibrational bands characteristic of amorphous and helical crystalline structure of the grafting copolymers are also highlighted.     

Simultaneous determination of naphazoline and pyridoxine in eye drops using excitation–emission matrix fluorescence coupled with second-order calibration method based on alternating trilinear decomposition algorithm

A novel method is developed for the direct determination of naphazoline hydrochloride(NAP) and pyridoxine hydrochloride(VB6) in commercial eye drops. By using excitation–emission matrix(EEM)fluorescence coupled with second-order calibration method based on the alternating trilinear decomposition(ATLD) algorithm, the proposed approach can achieve quantitative analysis successfully even in the presence of unknown and uncalibrated interferences. The method shows good linearity for NAP and VB6 with correlation coefficients greater than 0.99. The results were in good agreement with the labeled contents. To further confirm the feasibility and reliability of the proposed method, the same batch samples were analyzed by multiple reaction monitoring(MRM) based on LC–MS/MS method.T-test demonstrated that there are no significant differences between the prediction results of the two methods. The satisfactory results obtained in this work indicate that the use of the second-order calibration method coupled with the EEM is a promising tool for industrial quality control and pharmaceutical analysis due to its advantages of high sensitivity, low-cost and simple implementation.