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41.
Raman spectroscopy was applied for the direct non-destructive analysis of amiodarone hydrochloride (ADH), the active ingredient of the liquid formulation Angoron®. The FT-Raman spectra were obtained through the un-broken as-received ampoules of Angoron®. Using the most intense vibration of the active pharmaceutical ingredient (API) at 1568 cm−1, a calibration model, based on solutions with known concentrations, was developed. The model was applied to the Raman spectra recorded from three as-purchased commercial formulations of Angoron® having nominal strength of 50 mg ml−1 ADH. The average value of the API in these samples was found to be 48.56 ± 0.64 mg ml−1 while the detection limit of the proposed technique was found to be 2.11 mg ml−1. The results were compared to those obtained from the application of HPLC using the methodology described in the European Pharmacopoeia and found to be in excellent agreement. The proposed analytical methodology was also validated by evaluating the linearity of the calibration line as well as its accuracy and precision. The main advantage of Raman spectroscopy over HPLC method during routine analysis is that it is considerably faster and no solvent consuming. Furthermore, Raman spectroscopy is non-destructive for the sample. However, the detection limit for Raman spectroscopy is much higher than the corresponding for the HPLC methodology. 相似文献
42.
D. I. D'yachenko A. G. Mustafin V. V. Shereshovets N. N. Kabal'nova V. P. Kazakov I. B. Abdrakhmanov G. A. Tolstikov 《Russian Chemical Bulletin》1998,47(8):1611-1612
An unusual direction of the reaction of 2-(cyclopent-2-enyl)aniline hydrochloride with dimethyldioxirane was found: the formation
of two isomeric products,viz., 3- and 6-chloro-2-(cyclopent-2-enyl)anilines, was observed.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1654–1655, August, 1998. 相似文献
43.
建立了一种适用于分析冰毒杂质的方法,并分析其形成原因。将冰毒样品溶于1 mL 0.1 mol/L pH7.0的磷酸盐缓冲液(4份缓冲液1份10%Na2CO3),杂质用0.5 mL乙酸乙酯萃取。结果共有8种物质被检出。N-甲酰甲基安非他明、N-乙酰甲基安非他明在样品中出现,说明此批冰毒由苯丙酮(phenyl-2-propanone,P-2-P)经Leuckart法合成。N-乙基甲基安非他明的检出,则说明用于合成此批冰毒的P-2-P由苯甲醛和硝基乙烷合成。从实验结果看,该法可以满足冰毒杂质分析的需要,为分析冰毒杂质成分的成因、判断冰毒样品的合成路径提供重要信息。 相似文献
44.
金纳米微粒与盐酸氯丙嗪相互作用的共振Rayleigh散射光谱研究及其分析应用 总被引:2,自引:3,他引:2
在pH 1.8~3.3的酸性介质中,金纳米微粒本身有一定的共振瑞利散射(RRS)强度,但盐酸氯丙嗪本身的RRS强度十分微弱,当二者共存时,溶液的RRS强度显著增强并出现新的RRS光谱,在280~368 nm之间产生强烈的散射带,其最大散射波长位于368 nm,并在284、440、498 nm处有明显的散射峰。在一定条件下,盐酸氯丙嗪在0~0.08 mg/L范围内与ΔIRRS强度成正比,方法具有较高的灵敏度,对盐酸氯丙嗪的检出限(3σ)达到1.75μg/L。本文考察了反应体系的RRS光谱特征,研究了适宜的反应条件、影响因素及分析化学性质,研究了共存物质的影响,表明方法具有较好的选择性,据此发展了一种用金纳米微粒作RRS探针测定盐酸氯丙嗪的新方法。 相似文献
45.
K. Terada T. Masuda Y. Yoshihashi E. Yonemochi 《Journal of Thermal Analysis and Calorimetry》2006,85(3):675-680
Isothermal
microcalorimetry was used to evaluate excipient compatibility of solid dosage
form. Oxybutynin hydrochloride and cefaclor were used as model drugs for compatibility
test with excipients. The calorimetric data for compatibility test were compared
with those of HPLC data. Evaluation of compatibility between drug and excipient
of solid dosage form might be possible to use isothermal microcalorimetry
instead of conventional method. By using microcalorimetric method, the evaluation
of the compatibility between drug and excipient could be successfully performed
with a simple operation in a short time. The application of the isothermal
microcalorimetry would be useful for the screening test of the drug compatibility
with excipients. 相似文献
46.
The synthesis and full characterization of a number of amino acid and dipeptide derivatives with sulfur-containing side chains derived from ferrocene carboxylic acid and ferrocene-1,1′-dicarboxylic acid is presented. In particular, compounds Fc-CO-(Aaa)n-OMe (4) and Fe[C5H4-CO-(Aaa)n-OMe]2 (3) with (Aaa)n = Cys(Bzl) (a), Cys(Bzl)-Cys(Bzl) (b), Cys(p-OMe-Bzl) (c), Cys(p-OMe-Bzl)-Cys(p-OMe-Bzl) (d), Met (e), and Met-Met (f) were prepared. Also, the free acid derivatives Fe[C5H4-CO-Met-OH]2 (6e) and Fc-CO-Met-OH (7e) were prepared and characterized. The solid state structures of 3a, 4b, and 4e were determined by single crystal X-ray diffraction. Compound 3a shows a 1,3′ substitution pattern on the Cp rings in the solid state. Structures in solution were determined by NMR, IR and CD spectroscopy, with particular emphasis on the question of hydrogen bonding and helical chirality of the metallocene. As an example, the full assignment for the Cp signals in the disubstituted derivative 3a was achieved by simulation of the 1H NMR signals from the cyclopentadienyl ring in combination with 2D-NOESY spectra. In solution, 3a has the known 1,2′ substitution pattern, which is stabilized by intramolecular hydrogen bonds. 相似文献
47.
《Arabian Journal of Chemistry》2022,15(4):103712
Although recent decades have witnessed the synthesis of 1,3,4-thiadiazoles via phosphorus POCl3-promoted cyclization reaction, simultaneous access to 2-amino-1,3,4-thiadiazole and 2-amino-1,3,4-oxadiazole analogs remains unexpected and elusive. Herein, a detailed regiocontrolled synthesis of 2-amino-1,3,4-thiadiazoles in good to high yields with good regioselectivities from readily available thiosemicarbazides using POCl3 was disclosed. Meantime, to establish a comprehensive structure–activity relationship, 2-amino-1,3,4-oxadiazole derivatives as single regioisomers were prepared via EDCI·HCl-triggered cyclization of the thiosemicarbazide intermediates. The in vitro anti-influenza assays proved that the selected compounds with the pyrazine/pyridine ring exhibited certain inhibitory activities against influenza A virus strains A/HK/68 (H3N2) and A/PR/8/34 (H1N1) in MDCK cells. Among them, N-(adamantan-1-yl)-5-(5-(azepan-1-yl)pyrazin-2-yl)-1,3,4-thiadiazol-2-amine (4j) was the most active compound, and exhibited favorable activity with EC50 values of 3.5 μM and 7.5 μM, respectively. In addition, the molecular docking results explained the reason why compound 4j had dual inhibitory activity and revealed the reasonable binding mode of this compound with the M2-S31N and M2-WT ion channels. This compound had the potential to be further developed as an anti-influenza drug. 相似文献
48.
Anil Saikia 《Tetrahedron letters》2006,47(1):43-46
A novel one-pot synthesis of pyrazoles has been accomplished by the reaction of β-formyl enamides with hydroxylamine hydrochloride catalysed by potassium dihydrogenphosphate in acid medium. 相似文献
49.
50.
The chiral separation of trimetoquinol hydrochloride, which is a bronchodilator (Inolin), and three related compounds by micellar electrokinetic chromatography was investigated using a bile salt as a chiral surfactant. Enantiomers of these compounds, except laudanosoline, were successfully separated within 12 min using a separation tube of effective length 500 mm × 0.05 rum i.d. and a 0.05 M sodium taurodeoxycholate solution of pH 7.0. The observed theoretical plate numbers of the peaks were ca. 150000. Chiral recognition was affected by the structure of bile salts, the pH of the buffer solutions used and the structure of the solutes. Of four kinds of bile salts, successful chiral separation was achieved only using sodium taurodeoxycholate solution under neutral conditions. The method was applied to the optical purity determination of trimetoquinol hydrochloride. The effects of surfactant concentrations and some additives to the micellar solution are briefly described. 相似文献