流动注射-化学发光法测定盐酸地尔硫卓

发现了盐酸地尔硫卓在过硫酸钾-鲁米诺化学发光反应体系中的后化学发光反应.据此发现建立了利用后化学发光反应测定盐酸地尔硫卓的流动注射化学发光新方法.方法的线性范围为3.0×10-6～1.0×10-4 g/mL,检出限为3×10-7 g/mL,对6.0×10-5 g/mL的盐酸地尔硫卓标准溶液进行11次平行测定的相对标准偏差为1.6%.方法已用于盐酸地尔硫卓片剂中盐酸地尔硫卓含量的测定.     

流动注射化学发光法测定盐酸氟桂利嗪

在酸性条件下,盐酸氟桂利嗪与KMnO4反应可产生弱的化学发光,甲醛的存在对这一反应的化学发光强度具有增强作用。据此,优化了化学发光反应条件,建立了测定盐酸氟桂利嗪的流动注射化学发光分析法。该方法测定盐酸氟桂利嗪的线性范围为8.0×10-7~8.0×10-5g/mL,检出限为8×10-7g/mL,对1.0×10-5g/mL盐酸氟桂利嗪标准溶液进行11次平行测定的相对标准偏差为2.2%。方法已用于盐酸氟桂利嗪胶囊中盐酸氟桂利嗪的测定。     

K3Fe(CN)6-钙黄绿素体系后化学发光反应测定盐酸氯丙嗪

发现了盐酸氯丙嗪在K3Fe(CN)6-钙黄绿素化学发光反应体系中的后化学发光反应,优化了反应条件,建立了一种利用后化学发光反应测定盐酸氯丙嗪的流动注射化学发光分析法.方法的检出限为3×10-8/mL,相对标准偏差为2.0%(2.0×10-6 g/mL盐酸氯丙嗪,n=11),线性范围为1.0×10-7～1.0×10-5 g/mL.此法已用于盐酸氯丙嗪片剂中盐酸氯丙嗪含量的测定,结果与药典方法测定值一致.     

流动注射-化学发光法测定盐酸三氟拉嗪

根据盐酸三氟拉嗪能显著增强铁氰化钾-鲁米诺体系的化学发光强度,建立了测定盐酸三氟拉嗪的流动注射-化学发光分析法.方法的线性范围为1.0×10-6～2.0×10-5 g/mL,2.0×10-5～1.0×10-4g/mL,线性相关系数分别为0.9996 和0.9990,相对标准偏差为1.4%(p=1.0×10-5 g/mL...     

后化学发光法测定盐酸地芬尼多

本文研究了盐酸地芬尼多在N-氯代丁二酰亚胺(NCS)-荧光素化学发光反应体系中的后化学发光反应,并在研究反应的动力学性质、化学发光光谱、荧光光谱及其相关问题的基础上,探讨了反应机理;优化了反应条件,建立了一种测定盐酸地芬尼多的流动注射后化学发光方法.所建立方法的线性范围为6.0×10-9～1.0×10-9g/mL(r=0.9993),检出限为2×10-9g/mL,对5.0×10-8g/mL盐酸地芬尼多测定的相对标准偏差为2.5%(n=11).此法已用于血浆中盐酸地芬尼多含量的测定.     

流动注射协同化学发光法测定盐酸多巴胺

基于在碱性介质中,盐酸多巴胺和单宁协同促进KIO4氧化鲁米诺反应而产生发光,建立了流动注射化学发光法测定盐酸多巴胺的新方法。该方法测定盐酸多巴胺的线性范围为2.0×10-10～6.0×10-8g/mL,检出限为1.17×10-10g/mL,对于8.0×10-10g/mL盐酸多巴胺测定11次的相对标准偏差为1.92%。方法可应用于盐酸多巴胺注射液和尿样中盐酸多巴胺的测定。     

硫酸卡那霉素化学发光新方法的研究

在碱性溶液中,N-溴代丁二酰亚胺可以氧化曙红产生化学发光,硫酸卡那霉素的存在可以显著地增强这一反应的化学发光信号。基于此发现,优化了实验条件,建立了测定硫酸卡那霉素的流动注射化学发光新方法。方法测定硫酸卡那霉素的线性范围为1.0×10-7～2.0×10-5g/mL,检出限为6×10-8g/mL,相对标准偏差为1.3%(5.0×10-6g/mL硫酸卡那霉素溶液,n=11)。该方法已用于滴眼液中硫酸卡那霉素含量的测定。对化学发光反应的机理也进行了初步的探讨。     

流动注射后化学发光法测定Ca~(2+)

实验发现Ca2+在铁氰化钾-钙黄绿素化学发光反应体系中的后化学发光反应.优化了反应条件,建立了一种利用后化学发光反应测定Ca2+的流动注射化学发光分析法.方法的线性范围为1.0×10-6～1.0×10-4 g/mL,检出限为3.0×10-7 g/mL, 相对标准偏差为1.8%(2.0×10-5 g/mL Ca2+,n=11).此法已用于自来水中Ca2+含量的测定,结果与标准方法测定值一致.     

流动注射后化学发光法测定盐酸阿比朵尔

研究了盐酸阿比朵尔在鲁米诺-K3Fe(CN)6化学发光反应体系中的后化学发光反应. 据此建立了测定盐酸阿比朵尔的流动注射后化学发光分析法. 方法的线性范围为6.0×10-9～1.0×10-7 g/mL, 检出限(3σ)为2×10-9 g/mL. 对4.0×10-8 g/mL的盐酸阿比朵尔溶液连续11次平行测定, RSD=1.3%. 方法已用于盐酸阿比朵尔胶囊及尿样中盐酸阿比朵尔含量的测定. 在对这一后化学发光反应的动力学性质、化学发光光谱、紫外可见吸收光谱以及一些相关问题研究的基础上, 提出了可能的反应机理.     

高碘酸钾-鲁米诺后化学发光反应的研究——流动注射-后化学发光法测定异烟肼

实验发现了异烟肼在高碘酸钾-鲁米诺化学发光反应体系中的后化学发光反应。在对这一后化学发光反应的动力学性质、化学发光光谱、荧光光谱、紫外可见吸收光谱以及一些相关问题研究的基础上,讨论了其可能的反应机理;建立了利用此后化学发光反应测定异烟肼的流动注射化学发光新方法。方法的线性范围为1.0×10-9~4.0×10-7g/mL,检出限为6×10-10g/mL,对5.0×10-8g/mL的异烟肼进行11次平行测定的相对标准偏差为1.7%。此法已用于异烟肼片剂中异烟肼含量的测定,结果与药典法测定值一致。     

Spectrofluorimetric Determination of Chlorpromazine Hydrochloride and Thioridazine Hydrochloride

Abstract

Fluorescence spectroscopy was applied to the development of a sensitive and simple method for the determination of chlorpromazine HCl and thioridazine-HCl. The method is based upon development of an intense fluorescence using N-bromosuccinimide as the fluorogenic reagent. The produced fluorescence has very characteristic excitation and emission spectra and was stable for at least one hour. The results were reproducible and as little as 5 ng/ml chloropromazine HCl and 1 ng/ml thioridazine-HCl could be determined. The method was applied successfully to the analysis of various commercially available dosage forms. The obtained results were in good agreement with those of the official BP 93 procedures.     

Facile Syntheses of the Three Major Metabolites of Thioridazine

Efficient, mild syntheses of the three major metabolites 2 – 4 of the important antipsychotic drug thioridazine ( 1 ) have been developed. The cardiotoxic metabolite 2 with a ring sulfoxide moiety was prepared in 96% yield by oxidation of 1 with NaIO₄ under acidic conditions. Four different procedures were elaborated for the selective side‐chain sulfide oxidation of 1 to mesoridazine ( 3 ), giving rise to yields of up to 91%. Finally, sulforidazine ( 4 ) was synthesised via oxidation of the sulfoxide 3 in the presence of either KMnO₄ or t‐BuOOH under basic conditions. Except for the oxidation with t‐BuOOH, all reactions took place under mild conditions within a few minutes, were nicely reproducible, and afforded medium‐to‐high yields of the desired products, which could be readily purified by column chromatography.     

Electrochemical Studies and Selective Detection of Thioridazine Using a Carbon Paste Electrode Modified with ZnS Nanoparticles and Simultaneous Determination of Thioridazine and Olanzapine

A novel ZnS nanoparticle‐modified carbon paste electrode (ZnSNP‐MCPE) was fabricated and used to study the electrooxidation of thioridazine (TR) using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The determination conditions, such as accumulation time, pH of solution, and modifier amount were optimized. The mechanism of the electrooxidation process on the surface of the modified electrode was studied electrochemically. A linear range of 0.1–36.0 µM with detection limit of 65.0 nM was obtained for TR. In a mixture containing TR and olanzapine (OLZ), the DPV peaks of two compounds can be well separate from each other with a potential difference of 425 mV. Finally, this method was successfully applied to determinate the TR content in real samples.     

Application of Flow Injection Method for the Determination of Thioridazine

Abstract

A simple flow-injection spectrophotometric method for the determination of thioridazine is described. The method is based on the oxidation of thioridazine with phosphotungstic acid in hydrochloric acidic media. Concentrations of thioridazine in the range 10 – 60 ppm are determined with a relative standard deviation of 1.1%. The method was applied to the determination of thioridazine in pharmaceutical formulations.     

Thioridazine induces immediate and delayed erythema in photopatch test

Thioridazine is a phenothiazine derivative that has been used as an antipsychotic; it rarely causes photosensitization. However, we noticed that this drug induced an erythematous reaction in a photopatch test. Six volunteers were patch tested with various concentrations of thioridazine and irradiated with a range of UVA doses, and the time courses of the color of and blood flow to the test sites were monitored. The free-radical metabolites of thioridazine generated under UVA irradiation and its effects on ascorbate radical formation were examined with an electron paramagnetic resonance (EPR) spectrometer in vitro. As a result, immediate erythema developed during UVA irradiation in most subjects when 1% thioridazine was applied for 48 h and irradiation doses were higher than 4 J cm(-2). Another peak of erythematous reaction was observed 8-12 h after irradiation. The in vitro examination detected an apparent EPR signal, which appeared when 2 mM thioridazine in air-saturated phosphate buffer was irradiated with UVA, whereas this reaction was attenuated under anaerobic conditions. The EPR signal of the ascorbate radical was augmented under both aerobic and anaerobic conditions. Thioridazine-derived oxidants and/or thioridazine radicals generated during UVA irradiation seem to play an important role in this unique phototoxic reaction.     

碳纳米纤维糊电极电化学发光法测定甲硫哒嗪

制备了基于碳纳米纤维糊电极(CFPE)的新型电化学发光传感器.运用电化学方法对CFPE进行了表征,并考察了三联毗啶钉和甲硫哒嗪在此电极上的电化学行为和电化学发光行为.结果表明,该电极表现出很好的电化学活性和电化学发光响应.基于甲硫哒嗪对三联吡啶钉电化学发光的增强作用,建立了测定甲硫哒嗪的电化学发光新方法.实验考察了缓冲...     

盐酸l-麻黄碱异构化为盐酸d-伪麻黄碱的反应机理探讨

麻黄碱;乙酰化中间体;异构化机理;2d-nmr;绝对构型     

Simultaneous Spectrophotometric Determination of Imipramine Hydrochloride with Chlordiazepoxide and Nortriptyline Hydrochloride with Fluphenazine Hydrochloride

Spectrophotometry was used with multivariate calibration to simultaneously determine compounds in mixtures. Two antidepressant mixtures were investigated: imipramine hydrochloride and chlordiazepoxide and nortriptyline hydrochloride and fluphenazine hydrochloride. Considerable spectral overlap and large differences in component concentrations were challenges. Since this type of analysis is often performed using complex algorithms, a simple strategy was used here for the simultaneous determination of both mixture components by classical least squares, principal component regression, and partial least squares. Experimental design was used to select the optimum parameters including the wavelength range, sampling interval, software, and derivative order. Accuracy was enhanced by proper wavelength selection. In addition, derivatives of the raw spectra improved the selectivity. The standard deviation, deviation of mean recovery from 100%, and prediction ability of the models were used as the responses. In respect to these terms, first-order derivatization of the spectra and a sampling interval of 1?nm provided the best results. In particular, the low concentration compounds in the mixtures (chlordiazepoxide and fluphenazine) were determined more accurately with precision lower than 3%. The strategy was used for the quality control of pharmaceuticals containing the mixtures without chemical pretreatment.     

高效液相色谱法测定林可霉素利多卡因凝胶中盐酸利多卡因含量

建立了高效液相色谱法（HPLC）测定林可霉素利多卡因凝胶中盐酸利多卡因含量的方法.优化后的试验条件如下：色谱柱为Agilent 5 Tc-C18（2）（250 mm×4.6 mm,5 μm）,流动相为0.05 mol/L硼砂溶液（pH=6.0）-甲醇-乙腈（体积比为68：19：13）,紫外检测波长为214 nm,流速1.0 mL/min,柱温30℃,进样量20 μL.试验结果表明：利多卡因的线性范围为40.1~240.6 μg/mL（r =0.999 4）,加样回收率为97.6%.建立的方法操作简便,可用于制剂中盐酸利多卡因的质量控制.