Application of capillary zone electrophoresis to determine second-generation H1 antihistaminic drugs, loratadine and rupatadine

Abstract The second generation of H1 antihistamines from the piperidine group are often used for treating allergic diseases due to their action on histaminic receptors, the primary mediator of allergy. Moreover, the antihistamines have anti-inflammatory action, mediated through platelet-activating factor blocking activity. A simple and rapid capillary zone electrophoresis method was developed and validated for the determination of loratadine (LOR) and rupatadine (RUP) in tablets. The analyses were carried out using a fused silica capillary of 50.2 cm (40 cm effective length), 75 µm i.d. The background electrolyte was composed of boric acid 35 mmol/L, pH 2.5. Voltage of 20 kV, hydrodynamic injection of 3447.3 Pa for 3s, temperature at 25 ºC, and UV detection at 205 nm were applied. Electrophoretic separation was achieved at 1.8 and 2.8 min for RUP and LOR, respectively. The method was linear for both drugs in a range of 50.0 to 400.0 µg/mL (r>0.99). The limits of detection and quantification were 46.37 and 140.52 µg/mL, for LOR and 29.60 and 89.69 µg/mL for RUP respectively. The precision was less than 5.0 % for both drugs. The average recovery was approximately 100 %. The proposed novel method can significantly contribute to the rapid detection of counterfeit products and in quality control of drug products containing antihistamines

Prospective study on outcome and advantage of primary skin grafting in cases of avulsion scalp injury following trauma

Background: Traumatic avulsion injury poses severe risk as the overlying protective covering is lost and the raw tissue is exposed to the environment. Avulsion injuries involving the scalp are even more complicated to treat because of significant cosmetic concern involved. Aim of the study was to find a better solution than the existing method, we conducted a prospective study involving 13 patients with isolated traumatic scalp avulsion injury.Methods: This prospective study was conducted in Motilal Nehru Medical College and associated Swaroop Rani Nehru Hospital, Prayagraj,  after taking written and informed consents from the patients, between June 2017 and June 2019.These were divided into two groups (A and B) based on whether the underlying periosteum was intact or not.Results: Patients with intact periosteum (Group A) underwent primary thin thickness skin grafting within a few hours of their admission while the other group (Group B) was treated with a traditional conservative approach. We compared the results of both the groups and found that Group A patients not only had satisfactory graft uptake (≥85 TBSA) but also had significant decreased risk of infection, lesser hospital stay, overall decreased healthcare cost, better cosmoses and early return to routine activity.Conclusions: For the surgeon, this single step procedure is safe and technically easy. Thus this approach was found to be superior than the current traditional approach.

Decompression and Anterior Transposition of Ulnar Nerve in Prevention and Progression of Claw Hand Deformity in Leprosy

Leprosy is very common disease in India. It is known for its deformities and social problem associated with it. Our study was aimed to follow that surgical decompression and its anterior transposition of ulnar nerve prevents the progress of claw hand in leprosy. During last 20 years study was conducted at centers mentioned and statistic collected. It was found that all cases which did not responded to drugs or had deformity beforehand did responded to surgery and were made patient comfortable. Methods: ?. Results: ?. Conclusion: ?.

Detection of QTL for panicle architecture in F2 population of rice

Panicle traits are the most important agronomic characters which directly relate to yield in rice. Panicle length (PL) being one of the major components of rice panicle structure is controlled by quantitative trait loci (QTLs). In our research, conducted at Research Farm of SKUAST-J, crosses of parental lines K343 and DHMAS were made for generating F2 mapping population, which were then transplanted into the field using augmented design-I. The F2 population was used for phenotypic evaluation, development of linkage map and identification of QTLs on the chromosomes by using SSR markers. A total of 450 SSR markers were used for screening both the parents of which 53 highly polymorphic markers were selected and used for genotyping of 233 genotypes of F2population. Linkage map was generated using MAPMAKER/EXP3.0 software, seven linkage groups were found distributed on 11 chromosomes of rice. QTLs were detected using QTL Cartographer (v2.5) software. Based on 1000 permutation tests, a logarithm of odds (LOD) threshold value 2.0 and 3.0 was set. Composite interval mapping was used to map QTLs in populations derived from bi-parental crosses. The phenotypic data, genotypic data and the genetic linkage map generated identified total three QTLs of which one was identified for PL qPL2, located at 85.01 cM position with 2.1 LOD value and in between the marker intervals RM324–RM208, this QTL explained the phenotype variation by 4.36%. The other two QTLs were identified for spikelet density (SD) qSD3.1 and qSD3.2, located at 28.91 and 39.51 cM, respectively, both with a flanking marker RM6832 on chromosome 3. The LOD value and phenotypic variation explained for qSD3.1 and qSD3.2 was 3.00 and 3.25; 9.70 and 12.34% respectively. The reported QTLs identified in the study suggested a less diversity in the parents used and also the rejection of not so useful markers from the used set of markers for PL and SD.

Morel-Lavallee Lesion Of Lumbar Region

Morel-Lavallee lesion is a closed degloving injury characterized by post-traumatic separation of subcutaneous fat plane form underlying fascia, & thus created potential space being filled by fluid & debris of varying nature. Though originally described in the thigh, it has also been described in other anatomical sites including lumbar region. The lesion usually presents as compressible/fluctuant swelling at traumatic site. Most of patients present few days to few weeks after injury. However, patients with ignored slow growing painless lesions may present with long standing mass like lesions which may need open surgical intervention. Here, we present a case of long standing Morel-Lavallee lesion of lumbar region in a patient from remote village.

Physico-chemical And Microscopic Study Of Arjuna (terminalia Arjuna) Bark

In present study plant of Arjuna has been taken for physical and chemical analysis in terms of microtome of bark, powder study, loss on drying, ash values, extractive values, bulk density, Acid insoluble ash, Water-soluble Ash, Water-soluble extractive value, Alcohol-soluble extractive, pH range, TLC, Tapped density, Compressibility index, Hauser ratio, Angle of repose, Ultra violet fluorescence analysis of drug, etc. Physical and chemical analysis an important place in standardization of Ayurvedic drugs in order to make its global acceptability. The plant of Arjuna botanically named as Terminalia arjuna linn.; family Combretaceae, has traditionally been used to treat many diseases especially heart disease for centuries, that’s why it is called as “Guardian of the heartâ€. Transverse sections of Arjuna bark shows the calcium oxalate crystal, starch grains and lignified cells respectively shows that Xylem Vessels, Sclerenchymatous Fibers, Cork Cells, Tracheids, Sclereids, LOD value of the sample of Arjuna is 5.63%. According to result the Arjuna has three Rf vaule0.70, 0.42, 0.28 table1.4. Angle of repose of powder sample shows the flow of powder. The extractive value of Arjuna have different solvent like water, ethanol, isopropanol, acetone, chloroform, benzene, toluene, petroleum ether, hexsene are respectively 50.80, 41.07,30.37, 8.95, 0.96, 0.67, 0.52, 0.51, 0.46.

Simultaneous determination of abamectin homologs H 2 B 1a and H 2 B 1b in gel formulation by high performance liquid chromatography

ABSTRACT Abamectin is a drug with antiparasitic properties used in several pharmaceutical formulations. The objective of this research was to develop and validate a high performance liquid chromatographic (HPLC) method for quantification of the two abamectin homologs (H2B1a and H2B1b) in gel formulation. This HPLC method was validated using a LichroCart(r) 100 RP-18 (125 x 4 mm, 5 µm) column. The mobile phase contained of acetonitrile and water (95:5 v/v) with 1% acetic acid. The flow rate was 1.0 mL min-1 and UV detection was performed at 245 nm. Mobile phase solutions were prepared containing a nominal concentration 185.2 µg mL-1 H2B1a and 9.6 µg mL-1 H2B1b. The method displayed good linearity in the concentration range of 148.1 - 222.3 µg mL-1 and 7.7 - 11.5 µg mL-1, for H2B1a and H2B1b, respectively, with a correlation coefficient of (r)> 0.99 for both compounds, calculated by the least mean squares method. Detection limits (DLs) were 2.8 µg mL-1 and 1.2 µg mL-1 and quantitation limits (QLs) were 8.6 µg mL-1 and 3.8 µg mL-1, for H2B1a and H2B1b, respectively. The method is simple, economical and efficient for the quantitative determination of abamectin H2B1a and H2B1b homologs in pharmaceutical preparations.

Studies on Genetic Parameters to Improve the Genetic Architecture of Tomato (Solanum Lycopersicum L.).

Selection which is the basis of every breeding programme operates only on variation which is of genetic nature. A wide range of variability present in any crop always provides the better chances of selecting desired types. A field experiment was carried out at Vegetable Research Farm, Department of Horticulture, Institute of Agricultural Sciences, Banaras Hindu University during 2012 to evaluate the diverse genotypes of tomato. Analysis of variance indicated highly significant differences among the genotypes for all the characters. The highest GCV and PCV were observed with the character fruit yield per plant followed by number of seeds per fruit. Whereas, the lowest GCV and PCV were recorded by the character days to 50% fruiting followed by days to 50% flowering. The heritability estimates were high for all the characters except number of branches per plant which showed moderate heritability. The maximum heritability was observed for number of seeds per fruit and average fruit weight. High GCV and heritability coupled with high genetic advance was observed for fruit yield per plant followerd by number of seeds per fruit indicating that they are governed by additive genes and could be effectively improved through selection.

Simultaneous determination of ethinyl estradiol and drospirenone in oral contraceptive by high performance liquid chromatography

A simple, rapid, economical and reliable high performance liquid chromatographic method has been developed and successfully applied in simultaneous determination of ethinyl estradiol and drospirenone in coated tablets. The HPLC method was performed on a LiChroCART® 100RP column (125x4 mm i.d., 5 µm) with acetonitrile:water 50:50 (v/v) as mobile phase, pumped at a flow rate of 1.0 mL.min-1. The fluorescence detection for ethinyl estradiol was made at λex= 280 nm and λem= 310 nm and a UV detection for drospirenone was made at 200 nm. The elution time for ethinyl estradiol and drospirenone were 4.0 and 5.7 min, respectively. The method was validated in accordance to USP 34 guidelines. The proposed HPLC method presented advantages over reported methods and is suitable for quality control assays of ethinyl estradiol and drospirenone in coated tablets.

Um método simples, rápido, econômico e confiável foi desenvolvido empregando a cromatografia líquida de alta eficiência para a determinação simultânea de etinilestradiol e drospirenona em comprimidos revestidos. O método foi realizado utilizando coluna LiChroCART® 100RP (125 x 4 mm d.i., 5 µm), a fase móvel constituída de acetonitrila:água, 50:50 (v/v) com vazão de 1,0 mL.min-1. A detecção foi realizada empregando fluorescência em λex= 280 nm e λem= 310 nm para o etinilestradiol e na região de UV em 200 nm para a drospirenona. O etinilestradiol e a drospirenona tiveram tempo de retenção de 4,0 e 5,7 min, respectivamente. O método foi validado de acordo com as diretrizes da USP 34. O método proposto apresentou vantagens sobre os relatados na literatura e pode ser considerado adequado para o controle de qualidade do etinilestradiol e da drospirenona em comprimidos revestidos.

Interhemispheric subdural empyema

The authors describe two cases of interhemispheric subdural empyema. Both presented with fever, headache and seizures. Imaging revealed interhemispheric subdural empyema. Aspiration of empyema through a burr hole was done in both cases with good postoperative recovery

Comparative study on two rapid and sensitive methods for quantitative determination of tenoxicam in tablets

Tenoxicam, a piroxicam analogue, is an NSAID (Non-Steroid Antinflamatory Drug). It is used in the symptomatic management of musculoskeletal and joint disorders such as osteoarthritis and rheumatoid arthritis, and also in the short-term management of soft-tissue injury. Its quantitative determination in pharmaceutical formulations is important to guarantee the desired therapeutic effects. The objective of this research was to develop, validate and compare spectrophotometric and chromatographic methods in the quantitative determination of tenoxicam in tablet preparations. In this work, tablets containing 20.0 mg of tenoxicam from different origins were analyzed. The spectrophotometric method was validated using 0.1 mol/L NaOH as solvent and a signal at 368 nm was taken. The HPLC method was validated using Synergi Hydro-RP® C18 column (250x4.6 mm, 4 µm). The mobile phase was constituted of methanol-water (61:39 v/v) with pH adjusted to 2.5 with formic acid, at a flow rate of 1.0 mL/min. UV detection was made at 375 nm. All analyses were performed with a column temperature of 25 ºC ± 1. The calibration curves were linear over a concentration range from 4.0-24.0 µg/mL with a correlation coefficient better than 0.9999. The detection limit (DL) and quantitation limit (QL) were 0.25 µg/mL and 0.90 µg/mL for UV method and 0.35 µg/mL and 1.20 µg/mL for HPLC method respectively. The intra-day and inter-day precision expressed as RSD were below 2 percent for both methods. The mean recovery of tenoxicam was found to be in the range of 98.5-101.25 percent for UV method and 99.01-101.93 percent for HPLC method. The UV and HPLC methods were found to be rapid, precise and accurate. Statistically there was no significant difference between proposed UV spectrophotometric and HPLC methods.

Tenoxicam, um análogo de piroxicam, é um AINE (Antiinflamatório Não-Esteróide). ë usado no tratamento sintomático de doenças musculoesqueléticas das juntas, tais como osteoartrite e artrite reumatóide, e, também, no tratamento de danos dos tecidos moles. Sua determinação quantitativa em formulações farmacêuticas é importante para garantir os efeitos terapêuticos desejados. O objetivo dessa pesquisa foi desenvolver, validar e comparar métodos espectrofotométrico e cromatográfico na determinação quantitativa de tenoxicam em comprimidos. Neste trabalho, comprimidos contendo 20,0 mg de tenoxicam de diferentes procedências foram analisados. O método espectrofotométrico foi validado utilizando-se 0,1 mol/L de NaOH como solvente e se obteve sinal a 368 nm. O método por CLAE foi validado utilizando-se coluna Synergi Hydri-RP® C18 (250x4,6 nm, 4µm). A fase móvel constitui-se de metanol-água (61:39 v/v), com pH ajustado para 2,5 com ácido fórmico, e velocidade de fluxo de 1,0 mL/minuto. A detecção por UV foi efetuada a 375 nm. Todas as análises foram realizadas com temperatura de coluna a 25 ºC ± 1. As curvas de calibração foram lineares na faixa de concentração de 4,0 a 24,0 µg/mL, comcoeficiente de correlação melhor que 0,9999. O limite de detecção (LD) e o limite de quantificação (LQ) foram 0,25 µg/mL e 0,90 µg/mL e 1,20 µg/mL por CLAE, respectivamente. A precisão intra e inter-dia, expressa como RSD, foi abaixo de 2 por cento para ambos os métodos. A média de recuperação do tenoxicam ficou na faixa de 98,5 a 101,25 por cento para o método de UV, e 99,01 a 101,93, para a CLAE. Os métodos de UV e de CLAE mostraram-se rápidos, precisos e exatos. Estatisticamente, não se observou diferença significativa entre os métodos espectrofotométricos (UV) e CLAE.

Determination of optimum wavelength and derivative order in spectrophotometry for quantitation of hydroquinone in creams

UV derivative spectrophotometry was used for quantitative determination of hydroquinone in creams. The aim of this work was to investigate optimum wavelength and order of derivative, and to validate the proposed spectrophotometric method. The results of standard curves were calculated and statistically analyzed through the least squares method in the interval from 10.0 to 26.0 µg/mL, in the first, second, third and fourth order derivatives. The quantitative determination was carried out by using the zero-crossing (Z-C) and zero-peak (Z-P) methods. The proposed method is simple, of low cost and provides reliable results in order to be used in quality control of creams containing hydroquinone as active substance.

A espectrofotometria derivada no UV foi usada para a determinação quantitativa de hidroquinona em cremes. O objetivo desta pesquisa foi investigar o melhor comprimento de onda e a ordem da derivada, bem como validar o método proposto. Os resultados das curvas analíticas foram analisados estatisticamente pelo método dos mínimos quadrados no intervalo de 10,0 a 26,0 µg/mL, na primeira, segunda, terceira e quarta ordens da derivada. As determinações quantitativas foram realizadas utilizando os métodos "zero-crossing (Z-C)" e zero-pico (Z-P). O método proposto é simples, de baixo custo e fornece resultados confiáveis podendo ser usado no controle de qualidade de cremes contendo hidroquinona como substância ativa.

Cromatografia líquida com fase quiral aplicada na separação enantiomérica de fármacos cardiovasculares / Applied chiral phase liquid chromatography in enantiomeric separation of cardiovascular drugs

A maioria dos agentes terapêuticos, freqüentemente prescritos, é formulada e comercializada sob a forma racêmica, embora, para alguns deles, já tenha sido demonstrado que os efeitos farmacológicos e/ou tóxicos estejam relacionados apenas a um dos enantiômeros. Além disso, é conhecido o fato de que os enantiômeros podem apresentar perfis farmacocinéticos e farmacodinâmicos diferentes. Neste trabalho foram selecionados compostos que fazem parte de um importante grupo de fármacos muito empregados na terapêutica. São fármacos freqüentemente prescritos em doenças cardiovasculares. As separações enantioméricas diretas do atenolol, betaxolol, metoprolol e nadolol foram obtidas utilizando-se fase estacionária quiral do tipo carbamato de celulose tris-3,5-dimetilfenil, Chiralcel OD®, (250 x 4.6 mm, 10 æm). Os enantiômeros do pindolol foram separados com fase estacionária quiral derivada de dinitrobenzoil (DNB), a-Burke 2®, (250 x 4.6 mm, 10 æm). Os fármacos foram cromatografados à temperatura ambiente, com volume de injeção de 20 æL. A detecção foi efetuada em 276 nm exceto para o pindolol, que foi detectado em 220 nm. Os métodos propostos neste trabalho empregando CLAE-FEQs oferecem vantagens sobre as técnicas clássicas de separação de enantiômeros e podem ser empregados na análise quantitativa dos enantiômeros em preparações farmacêuticas e amostras biológicas.

The majority of frequently prescribed therapeutic agents are formulated and commercialized in the racemic form, even though, for some of them, it has already been demonstrated that the pharmacological and/or toxicological effects are associated only with one of the enantiomers. Moreover, it is well known that these antipodes can present different pharmacokinetic and pharmacodynamic profiles. In this work we selected drugs that belong to an important group of pharmaceuticals, frequently prescribed in the treatment of cardiovascular disorders. The direct enantiomeric separations of atenolol, betaxolol, metoprolol and nadolol were obtained using the chiral stationary phase cellulose tris-3,5-dimethylphenyl-carbamate, Chiralcel OD® (250 x 4,6 mm, 10 æm). The enantiomers of pindolol were separated with the chiral stationary phase derived from dinitro-benzoyl (DNB) (S, S) alpha-Burke 2® (250x4.6 mm, 10 æm). The drugs were chromatographed at room temperature, with injection volumes of 20 æL. The detention was made at 276 nm except for pindolol, which was detected at 220 nm. The proposed methods in this work using HPLC-CSP offer advantages over contemporaneous techniques of enantiomeric separation, being rapid and efficient, and can be used in the simultaneous quantitative analysis of referred enantiomers in pharmaceutical preparations and biological samples.

First-derivative ultraviolet spectrophotometric and high performance liquid chromatographic determination of ketoconazole in pharmaceutical emulsions

Foram desenvolvidos e padronizados métodos por espectrofotometria no ultravioleta (UV) por derivada de primeira ordem (Método I) e cromatografia líquida de alta eficiência (CLAE) (Método II) para a determinação quantitativa de cetoconazol em formulações farmacêuticas sob a forma de emulsão obtida no comércio e formulada em laboratório. A espectrofotometria no UV por derivada de primeira ordem foi padronizada usando-se o método do zero pico a 257 nm, utilizando metanol como solvente. A cromatografia líquida foi realizada empregando-se uma coluna LiChrospher® 100 RP-18 (5 µm). A fase móvel utilizada foi a mistura de trietilamina em metanol (1:500) e solução de acetato de amônio em água (1:200) na proporção de 75:25 v/v, com vazão de 1 mL/min e detecção no UV de 225 nm. O tempo de retenção do cetoconazol foi de 3,9 min e do terconazol de 5,9 min, este último utilizado com padrão interno. As curvas analíticas mostraram linearidade dentro das concentrações de 5,0 a 30,0 µg/mL para o Método I e 20,0 a 80,0 µg/mL para o Método II, com coeficientes de correlação linear de 0,9997 e 0,9981, respectivamente.O desvio padrão relativo (DPR) foi de 0,56% e 0,41% para a amostra simulada e comercial, respectivamente, empregando-se o Método I. Para o Método II, os valores foram de 2,13% e 1,25%, respectivamente. A porcentagem de recuperação foi de 100,1% para o Método I e 100,4% para o Método II. Os excipientes não interferiram nas análises. Os resultados mostraram que os dois métodos podem ser usados para a determinação rápida de cetoconazol em formulações de emulsões com precisão, exatidão e especificidade.

Quantitative determination of ciprofloxacin and norfloxacin in pharmaceutical preparations by high performance liquid chromatography

The objetive of the research was to develop and validate an analytical method for quantitative determination of ciprofloxacin (CIP) and norfloxacin (NOR) in pharmaceutical preparations. A simple and rapid chromatographic method was developed and validated for quantitative determination of two fluoroquinolone antibiotics in tablets and injection preparations. The quinolones were analyzed by using a LiChrospher® 100 RP-18 column (5 µm, 125 x 4 mm) and a mobile phase consisted of water:acetronitrile:triethylamine (80:20:0.3 v/v/v). The pH of final mixture was adjusted to 3.3 with phosphoric acid. The flow rate was 1.0 mL/min and UV detection was made at 279nm. The analyses were performed at room temperature (24 ± 2°C). CIP and NOR were eluted within 5 min. The calibration curves were linear (r > 0.9999) over a concentration range from 4.0 to 24.0 µg/mL. The relative standard deviation (RSD) was < 1.0 percent and the mean recovery was 101.85 percent...

Validação de um método analítico para a determinação de substâncias ativas em formulações farmacêuticas empregadas em ®peelings¼ químicos / Validation of analytical methods for the determination of active substances in pharmaceutical preparations used in chemical peelings

Nos "peelings" químicos utilizam-se formulações esfoliantes, empregadas na terapêutica de queratoses actínicas, rugas, discromias pigmentares, acne vulgar e rosácea. Na presente pesquisa, foram empregadas como amostras, a solução de Jessner (SJ) composta por resorcinol (RS) 14 por cento e ácido láctico (AL) 14 por cento em solução alcoólica e géis de AS a 20 por cento e RS a 30 por cento. As técnicas utilizadas foram a espectrofotometria derivada no UV de primeira e segunda ordens em etanol absoluto para o AS e RS, respectivamente na SJ, e a espectrofotometria derivada no UV de primeira ordem em ácido sulfúrico 0,1 N para o AS e RS nos géis. Para o AS na SJ, o coeficiente de correlação (r) foi de 0,9999, a precisão expressa pela média dos desvios padrão relativos (DPR) de 0,68 por cento e a exatidão expressa pela recuperação média de 100,5 por cento...

Separação enantiomérica de fármacos em medicamentos por cromatografia líquida com fase estacionária quiral / Enantiomeric separation of drugs in medicine by liquid chromatography with chiral stationary phase

A maioria dos agentes terapêuticos, freqüentemente prescritos, são formulados e comercializados sob a forma racêmica, embora para alguns deles, já tenha sido demonstrado que os efeitos farmacológicos e/ou tóxicos estejam relacionados apenas a um dos enantiômeros. Além disso, é conhecido o fato de que os enantiômeros podem apresentar perfis farmacocinéticos e farmacodinâmicos diferentes. Neste trabalho foram selecionados fármacos que fazem parte de dois grupos importantes no uso clínico. São fármacos freqüentemente prescritos, como os BETA-bloqueadores (atenolol, metoprolol, pindolol, betaxolol e nadolol) e os antiinflamatórios não-esteróides (ibuprofeno e flurbiprofeno)...

Development and regulation of chiral drug substances: an overview on worldwide pharmaceutical guidelines

Optical rotation, the ability of a substance to rotate the plane of the polarized light, was known since 1815. The proposal of Louis Pasteur in 1848 made it clear that the optical activity of organic solution is determined by molecular asymmetry, wich produces non-superimposable mirror-image structures (Drayer, 1993). Since discovery and exploitation of chiral pharmaceuticals for clinical use, major advances have been made regarding stereoselective pharmacological activity, differential pharmacokinetics, pharmacodynamics profiles, their toxicological divergences and recently economical interests. These factors made it necessary the drug authorities of several countries to publish and adopt guidelines...