Comparative Analysis of Lonicera japonica Flower from Different Harvesting Periods Based on UV Fingerprint and Chemometrics / 中国实验方剂学杂志

ObjectiveTo investigate the quality variation of Lonicera japonica flower from different harvesting periods by ultraviolet visible（UV-Vis） fingerprint combined with chemometrics. MethodTwenty-five L. japonica flower samples from five harvesting periods， including young bud stage，green bud stage，white bud stage，silver and golden flower stages， were collected， with five samples for each stage. UV-Vis fingerprints of L. japonica flower from different harvesting periods were established in the context of the optimum extraction method based on the single factor experiment. The results showed that the absorption values at 209，216，226，250，280，303，318， and 350 nm were significantly different. Moreover，after data pretreatment and normalization，multivariate statistical analyses， such as principal component analysis （PCA），partial least squares discriminant analysis （PLS-DA），and orthogonal PLS-DA （OPLS-DA）were performed by SIMCA-P+ to establish the quality variation model of L. japonicas flower from harvesting periods. ResultAs revealed by PCA and PLS-DA， L. japonicas flower samples from five harvesting periods were clustered separately and closely in a harvesting time-dependent manner， suggesting that the content of components contained in samples from different harvesting periods was highly distinct and correlated with harvesting periods. The pairwise comparison of OPLS-DA indicated that triterpenoids or volatile oils were the main components causing the changes from the young bud stage to the green bud stage，and the content of them decreased. The main components from the green bud stage to the white bud stage were triterpenoids （or iridoids），volatile oils，phenolic acids， or flavonoids，and the content of them decreased， which was consistent with the HPLC result of chlorogenic acid. From the white bud stage to the silver flower stage， the main components were iridoids （increasing in content） and triterpenoids （or volatile oils） （decreasing in content）. The main altered components from the silver flower stage to the golden flower stage were triterpenoids （or volatile oils） whose content increased. ConclusionThis method is simple and feasible， which can provide references for the quality control of Chinese medicine.

Development and validation of an UV-Vis spectrophotometric method for the quantification of oclacitinib in capsule formulation

Objective. The aim of this study was the development and validation of an UV-Vis spectrophotometric method for the quantification of oclacitinib in commercial capsule formulation since pharmacopeias have not yet provided an official monograph for this drug. Methods. The parameters linearity, limit of detection, limit of quantitation, specificity, precision, accuracy, and robustness were determined according to Brazilian and international guidelines. Results. Linearity was determined for the analytical range of 5-15 µg/mL, and a limit of detection of 1.18 µg/mL and limit of quantification of 3.58 µg/mL were obtained. The method was selective and the precision was demonstrated through repeatability and intermediate precision, with relative standard deviations of 1.96% and 1.78%, respectively. In its turn, accuracy presented recovery percentages of 98.32-100.91%. All robustness and sample stability (48 h at 25 °C) results revealed no statistical variation among the groups. Conclusions. The presented method is suitable for the quantification of oclacitinib in commercial capsule formulation.

A dual-signal sensor for the analysis of parathion-methyl using silver nanoparticles modified with graphitic carbon nitride / 药物分析学报

A highly sensitive and selective method was developed for both UV-vis spectrophotometric and fluo-rimetric determination of organophosphorus pesticides(OPs).This method used silver nanoparticles(AgNPs)modified with graphitic carbon nitride(g-C3N4).The AgNPs reduced the fluorescence intensity of g-C3N4.Acetylthiocholine(ATCh)could be catalytically hydrolyzed by acetylcholinesterase(AChE)to form thiocholine,which induces aggregation of the AgNPs.This aggregation led to the recovery of the blue fluorescence of g-C3N4,with excitation/emission peaks at 310/460 nm.This fluorescence intensity could be reduced again in the presence of OPs because of the inhibitory effect of OPs on the activity of AChE.The degree of reduction was found to be proportional to the concentration of OPs,and the limit of fluorometric detection was 0.0324 μg/L(S/N = 3).In addition,the absorption of the g-C3N4/AgNPs at 390 nm decreased because of the aggregation of the AgNPs,but was recovered in presence of OPs because of the inhibition of enzyme activity by OPs.This method was successfully applied to the analysis of parathion-methyl in real samples.

Use of different matrices to construct the standard curve for the paracetamol dosage by visible spectrophotometry / Uso de diferentes matrizes na construção da curva padrão para a dosagem de paracetamol por espectrofotometria visível

ABSTRACT Introduction: Acute paracetamol poisoning is confirmed by the determination of its serum level and allows assessing the risk of hepatotoxicity, which can be monitored by the Rumack-Matthew nomogram for the administration of the N-Acetylcysteine antidote, as well as for the prognosis of intoxication. Objective: Because of its analytical importance, we evaluated the influence of different matrices (ultrapure water, serum, and plasma) on the construction of the paracetamol calibration curve, aiming to reduce the analytical cost and facilitate its implementation in clinical and emergency laboratories. Material and methods: A standard stock solution of paracetamol of 1 mg ml-1 was obtained, from which appropriate dilutions originated the following concentrations 20, 50, 100, 150, 200, 250, and 300 mg l-1 in the different matrices, in triplicate, reading at complete after 430 nm in spectrophotometer and reproduced after three months. The results were statistically analyzed (p < 0.05). Results and discussion: Good laboratory practices include remaking the calibration curve when stock reagents are remade aiming to readjust the line equation indicated by a measuring instrument. The biological samples indicated as matrices on a calibration curve are usually serum and plasma. However, these biological products, when commercially purchased, are of high cost. Ultrapure water can replace serum and plasma in the paracetamol calibration curve according to the linearity of the curve, which showed the same trend line for the three matrices. Conclusion: The three matrices can be used in the construction of the paracetamol calibration curve, but the use of ultrapure water reduces the analysis costs.

RESUMEN Introducción: La intoxicación aguda por paracetamol se confirma mediante la determinación de su nivel sérico y permite evaluar el riesgo de hepatotoxicidad, que puede ser monitorizado mediante el nomograma de Rumack-Matthew para la administración del antídoto N-acetilcisteína, así como para el pronóstico de intoxicación. Objetivos: Por su importancia analítica, se evaluó la influencia de diferentes matrices (agua ultrapura, suero y plasma) en la construcción de la curva de calibración del paracetamol, con el objetivo de reducir el costo analítico y facilitar su implementación en laboratorios clínicos y de emergencia. Material y métodos: Se obtuvo una solución madre del estándar (stock) de paracetamol de 1 mg ml-1, de la cual se originaron diluciones adecuadas para obtener las siguientes concentraciones de 20, 50, 100, 150, 200, 250 y 300 mg l-1 con las diferentes matrices, por triplicado, con lectura a 430 nm en epectrofotômetro, reproduciéndose a los tres meses. Los resultados se analizaron estadísticamente (p < 0,05). Resultados y discusión: Las buenas prácticas de laboratorio incluyen rehacer la curva de calibración cuando se rehacen los reactivos del estándar con el fin de reajustar la ecuación lineal indicada por un instrumento de medición. Las muestras biológicas indicadas como matrices en una curva de calibración suelen ser suero y plasma. Sin embargo, estos productos biológicos cuando se compran comercialmente son de alto costo. El agua ultrapura puede reemplazar el suero y el plasma en la curva de calibración de paracetamol de acuerdo con la linealidad de la curva, que mostró la misma línea de tendencia para las tres matrices. Conclusión: Las tres matrices pueden usarse en la construcción de la curva de calibración de paracetamol, pero el uso de agua ultrapura reduce los costos de análisis.

RESUMO Introdução: A intoxicação aguda pelo paracetamol é confirmada pela determinação de seu nível sérico e permite avaliar o risco de hepatotoxicidade, que pode ser monitorado pelo nomograma Rumack-Matthew para a administração do antídoto N-acetilcisteína, bem como para o prognóstico da intoxicação. Objetivos: Diante de sua importância analítica, avaliamos a influência de diferentes matrizes (água ultrapura, soro e plasma) na construção da curva de calibração do paracetamol, visando diminuir o custo analítico e facilitar a sua implantação em laboratórios clínicos e de urgência. Material e métodos: Obtivemos uma solução estoque padrão de paracetamol de 1 mg ml-1, da qual originaram diluições apropriadas para se obter as concentrações de 20, 50, 100, 150, 200, 250 e 300 mg l-1 com as diferentes matrizes, em triplicata, com leituras em espectrofotômetro a 430 nm, sendo reproduzidas após três meses. Os resultados foram analisados estatisticamente (p < 0,05). Resultados e discussão: Nas boas práticas de laboratório, inclui-se o refazimento da curva de calibração quando os reagentes estoques são refeitos visando ao reajuste da equação de reta indicado por um instrumento de medição. As amostras biológicas indicadas como matrizes em uma curva de calibração são, usualmente, soro e plasma. Porém, esses produtos biológicos quando adquiridos comercialmente são de custo elevado. A água ultrapura pode substituir soro e plasma na curva de calibração do paracetamol em função da linearidade da curva, a qual mostrou a mesma linha de tendência para as três matrizes. Conclusão: As três matrizes podem ser utilizadas na construção da curva de calibração do paracetamol, mas o uso de água ultrapura diminui os custos da análise.

Determination of shelf life of four herbal medicinal products using high-performance liquid chromatography analyses of markers and the Systat Sigmaplot software

Shelf life determination of herbal medicines is of paramount importance as it relates to activity of constituents of theproduct. This work sought to determine shelf life of four herbal products (Nibima, Asena, Lippia tea, and NPK 500capsules). The method involved the determination of marker content of products (three batches each) at time points(0, 3, 6, 9, 12, and 18 months) at storage temperature and humidity of 30°C ± 2°C/70% RH ± 5% RH using highperformance liquid chromatography (HPLC) analyses. Batch blending was employed for preparation of referencesamples of products. In UV analyses, λmax of 289, 291, 327, and 289 nm were obtained from spectra for (Nibima,Asena, Lippia tea, and NPK 500 capsules, respectively. A common 230 nm UV marker was observed for all theproducts. Optimized HPLC conditions were developed for products using methanol: water: 0.1%v/v acetic acidsystem with mobile phase ratios of 9:0:1 (Nibima), 7:2:1 (Asena), 8:1:1 (Lippia tea), and 90:5:5 (NPK 500 capsules).Wavelength of detection used for HPLC analyses were 283, 290, 332, and 290 nm for Nibima, Asena, Lippia tea, andNPK 500 capsules, respectively. HPLC marker content analyses with time produced shelf life of 23.14, 21.16, 62.97and 32.91 months for Nibima, Asena, Lippia tea, and NPK 500 capsules, respectively. Obtained shelf life indicatesrelative stability of products.

Quantification of biogenic amines in fabrication steps of Gorgonzola-type cheese / Quantificação de aminas biogênicas nas etapas de fabricação do queijo tipo Gorgonzola

During the Gorgonzola-type cheese preparation there are proteolysis and lipolysis which may be influenced by the type of starter culture chosen. Six manufacturing steps were selected to identify which of them is most suitable for biogenic amines (BA) formation (1- milk, 2- lactic acid bacterial culture and fungus addition, 3- curd, 4- dry salting, 5- maturation at 30 days and maturation at 60 days); perform research on enterobacteria; accomplish the research of BA-producing bacteria (BAPB); detect and quantify the most abundant BA (putrescine, cadaverine, tyramine, histamine, spermidine and spermine) in the six steps of Gorgonzola cheese production and in bacterial isolates using high performance liquid chromatography and UV-Vis SPD/10AV detector and define if the presence of enterobacteria and BAPB would be correlated with BA production in this cheese. The bacterial culture used increased its log population by 7 log cycles and reached its highest level in batch 2 during cheese maturation. There was a decrease in the enterobacterial population in 2 log cycles after 60 days of maturation in batch 1. Tyramine was the BA with the highest concentration 306.32 mg.Kg-1 quantified in step 6 (60 days maturation) in batch 1. Criterion is requiered in bacterial starter culture selection because it is a quality determinant factor in relation to BA production and more rigor in raw material selection.

Durante a elaboração do queijo tipo Gorgonzola ocorre proteólise a partir das bactérias e dos fungos adicionados ao leite que podem levar a formação de aminas biogênicas (AB) neste tipo de queijo. Portanto, no presente estudo foi feito o acompanhamento com coleta de amostras em seis etapas na fabricação deste queijo paraidentificar em qual delas haveria maior formação de aminas biogênicas (AB). As amostras coletadas em três diferentes lotes foram o leite cru (1), leite pasteurizado adicionado de cultura de bactérias ácido-láticas (2), massa coalhada (3), queijo após a etapa de salga seca (4), queijo após 30 dias de maturação (5) e queijo após 60 dias de maturação (6). Também foram realizadas a pesquisa de enterobactérias e bactérias ácido-láticas com característica capacidade de descarboxilação de aminoácidos e produção de aminas biogênicas (BPAB); detecção e quantificação da AB mais abundante (putrescina, cadaverina, tiramina, histamina, espermidina e espermina) nas seis etapas de fabricação do queijo tipo Gorgonzola e nos isolados bacterianos utilizando cromatografia líquida de alta eficiência e detector UV-Vis SPD/10AV e a verificação se a presença de enterobactérias e BPAB estariam correlacionadas com a produção de AB nesse queijo. A cultura bacteriana utilizada cresceu aumentando em sete ciclos logarítmicos sua população e alcançou seu maior nível no lote 2 na etapa de maturação do queijo. Houve diminuição da população enterobactérias em 2 ciclos logarítmicos após 60 dias de maturação no lote 1. A tiramina foi a AB com concentração mais elevada 306,32 mg.Kg-1 quantificada na etapa 6 (60 dias de maturação) no lote 1. É necessário dar mais atenção em duas etapas na elaboração dos queijos: mais critério na seleção da cultura bacteriana iniciadora por ser um fator determinante na qualidade em relação à produção de AB e mais rigor na seleção da matéria-prima.Palavras chaves: cromatografia, cultura iniciadora, detector SPD/10AV UV­Vis, maturação, tiramina.

Content determination of total flavones and polysaccharides in Fangshu Qingre mixture by UV-Vis spectrophotometry / 药学实践杂志

Objective To establish a method for content determination of total flavones and polysaccharides in Fangshu Qingre mixture by UV-Vis Spectrophotometry. Methods The contents of total flavones and polysaccharides in Fangshu Qingre mixture were determined by UV-Vis spectroscopy with rutin and anhydrous glucose as reference substance, and the wavelength was set at 508 nm and 487 nm. Results The contents were from 0.00 to 59.20 μg/ml for total flavones and from 10.92 to 109.20 μg/ml for total polysaccharides in Fangshu Qingre mixture. The recoveries of total flavones and total polysaccharides were 104.4% and 104.8% respectively. Conclusion The method of using ultraviolet spectroscopy was simple, reproducible, accurate and reliable, which could be preferably used as the method for content determination of total flavones and polysaccharides in Fangshu Qingre mixture.

Study on rapid quality analysis method of Shengxuebao Mixture / 中国中药杂志

A rapid analysis method based on ultraviolet-visual(UV-Vis) spectroscopy, near infrared(NIR) spectroscopy and multivariable data analysis was established for quality evaluation of Shengxuebao Mixture. The contents of eight active ingredients of Shengxuebao Mixture including albiflorin, paeoniflorin, 2, 3, 5, 4'-tetra-hydroxy-stilbene-2-O-β-D-glucopyranoside, specnuezhenide,ecliptasaponin D, emodin, calycosin-7-glucoside and astragaloside Ⅳ were simultaneously detected by using this method. HPLC-UV-MS was used as a reference method for determining the contents of these ingredients. Partial least squares(PLS) analysis was implemented as a linear method for multivariate models calibrated between UV spectrum/NIR spectrum and contents of 8 ingredients. Finally, the performance of the model was evaluated by 24 batches of test samples. The results showed that both UV-Vis and NIR models gave a good calibration ability with an R~2 value above 0.9, and the prediction ability was also satisfactory, with an R~2 value higher than 0.83 for UV-Vis model and higher than 0.79 for NIR model. The overall results demonstrate that the established method is accurate, robust and fast, therefore, it can be used for rapid quality evaluation of Shengxuebao Mixture.

Synthesis and Characterization of Silver Nanoparticles from Ethanolic Extracts of Leaves of Annona muricata: A Green Nanobiotechnology Approach

Introduction: The biological green synthesis of nanoparticles via nanobiotechnology processes have a significant potential to boost nanoparticles production without the use of harsh, toxic, and expensive chemicals commonly used in conventional physical and chemical processes. Annona muricata, a tropical plant belonging to family Annonaceae is one of the most used plants in folk medicine because of its many medicinal uses and therefore presents a strong candidate for use in green synthesis. Aims: The aim of this study was to optimize a method for the synthesis of Silver Nanoparticles (AgNPs) from ethanolic extracts of leaves of Annona muricata as well as to characterize the green synthesized AgNPs. Methodology: AgNPs were synthesized from Annona muricata leaves using AgNO3 solution. The AgNPs were characterized using spectroscopy and microscopy techniques. Results: The formed AgNPs had an absorption maximum at 429 nm using UV–Visible spectroscopy and were stable under different pH, temperature, and storage conditions. Fourier transform infrared analysis revealed the different functional groups responsible for the synthesis and stabilization of the AgNPs. Scanning electron microscopy analysis revealed a spherical nature of the synthesized AgNPs. Energy dispersive x-ray spectroscopy analysis showed presence of Ag, O, and Cl with Ag having the highest composition at 60%. X-Ray Diffraction and Dynamic Light Scattering revealed a crystalline nature of AgNPs with an average size of 87.36 nm and a polydispersity index of 0.16 respectively. Transmission Electron Microscopy analysis further confirmed the crystalline and spherical nature of the AgNPs. Conclusion: In this article, an efficient, eco-friendly and low-cost method for the synthesis and recovery of stable AgNPs using Annona muricata leaves ethanolic extracts as both a reducing and capping agent has been reported for the first time. The synthesized AgNPs could be promising candidates for many biomedical, clinical, engineering, and polymer applications.

Synthesis, characterization, and in vitro evaluation of gamma radiationinduced PEGylated isoniazid

Background: The search for innovative anti-tubercular agents has received increasing attention in tuberculosis chemotherapy because Mycobacterium tuberculosis infection has steadily increased over the years. This underlines the necessity for new methods of preparation for polymer-drug adducts to treat this important infectious disease. The use of poly(ethylene glycol)(PEG) is an alternative producing anti-tubercular derivatives. However, it is not yet known whether PEGylated isonicotinylhydrazide conjugates obtained by direct links with PEG are useful for therapeutic applications. Results: Here, we synthesized a PEGylated isoniazid (PEG-g-INH or PEG­INH) by gamma radiation-induced polymerization, for the first time. The new prodrugs were characterized using Raman and UV/Vis spectrometry. The mechanism of PEGylated INH synthesis was proposed. The in vitro evaluation of a PEGylated isonicotinylhydrazide macromolecular prodrug was also carried out. The results indicated that PEG­INH inhibited the bacterial growth above 95% as compared with INH, which showed a lower value (80%) at a concentration of 0.25 µM. Similar trends are observed for 0.1, 1, and 5 µM. Conclusions: In summary, the research suggests that it is possible to covalently attach the PEG onto INH by the proposed method and to obtain a slow-acting isoniazid derivative with little toxicity in vitro and higher antimycobacterial potency than the neat drug.

Formulation and pharmacopoeial quality evaluation of ketorolac tromethamine IR tablet and comparison with marketed product

This study describes the formulation of immediate release Ketorolac tromethamine (KT) 10-mg tablet by directcompression method; evaluation of their compliance to various Pharmacopoeial quality parameters, i.e., weightvariation, friability, hardness, thickness, moisture content, disintegration, assay, and dissolution; and their comparisonwith marketed brands for determination of pharmaceutical equivalency. Five formulations of KT were prepared(coded as FKT1, FKT2, FKT3, FKT4, and FKT5) by direct compression method using different superdisintegrants.Micrometric properties of the mixtures of the drug and the excipients prepared for formulation were evaluated. Qualityevaluation of the five different formulations and randomly selected four different brands of KT 10-mg tablets purchasedfrom the local market (coded as LKT1, MKT2, MKT3, and SKT4) were performed according to Pharmacopoeia. Theresults were obtained by UV-Vis spectrophotometer and all the dissolution profiles were characterized by the zeroorder kinetics. All the brands of KT and developed formulations met the official specification except SKT4 whichshowed excessive moisture content of 7.18%. None of the tested brands of KT were found to be pharmaceuticallyequivalent, whereas two developed formulation were pharmaceutically equivalent with the in house benchmark(MKT2) from which their interchangeability can be suggested.

Development and validation of spectrophotometric method for determination of gabapentin in bulk and pharmaceutical dosage forms based on Schiff base formation with salicylaldehyde

A sensitive, simple, and economic spectrophotometric method was developed and validated for the determination ofgabapentin in pure form and pharmaceutical preparations. The method is based on Schiff base condensation reaction ofthe primary amino group of gabapentin with salicylaldehyde reagent in the presence of acetate solution at 45°C for 20minutes. The obtained yellow-colored derivative in methanolic medium showed absorption maxima at 403 nm. Underthe optimum conditions, Beer’s law was obeyed in the concentration range of 6 to 100 μg/ml with correlation coefficientvalue of 0.9961. Limit of detection and limit of quantification were found to be 1.16 and 3.48 μg/ml, respectively. Thevalidity of the described method was assessed according to the International Conference on Harmonization guidelines.The mean percentage recoveries ± SD were 100.57 ± 1.5 by applying the standard addition technique. The method wasrepeatable and precise (RSD ≤ 0.61% and ≤ 1.34%, respectively) and was successfully applied for the determinationof the investigated drug in its pharmaceutical dosage form without detectable interference from the additives, hence,can be suggested for routine analysis of the gabapentin.

Development and validation of spectrophotometric method for determination of gabapentin in bulk and pharmaceutical dosage forms based on Schiff base formation with salicylaldehyde

A sensitive, simple, and economic spectrophotometric method was developed and validated for the determination ofgabapentin in pure form and pharmaceutical preparations. The method is based on Schiff base condensation reaction ofthe primary amino group of gabapentin with salicylaldehyde reagent in the presence of acetate solution at 45°C for 20minutes. The obtained yellow-colored derivative in methanolic medium showed absorption maxima at 403 nm. Underthe optimum conditions, Beer’s law was obeyed in the concentration range of 6 to 100 μg/ml with correlation coefficientvalue of 0.9961. Limit of detection and limit of quantification were found to be 1.16 and 3.48 μg/ml, respectively. Thevalidity of the described method was assessed according to the International Conference on Harmonization guidelines.The mean percentage recoveries ± SD were 100.57 ± 1.5 by applying the standard addition technique. The method wasrepeatable and precise (RSD ≤ 0.61% and ≤ 1.34%, respectively) and was successfully applied for the determinationof the investigated drug in its pharmaceutical dosage form without detectable interference from the additives, hence,can be suggested for routine analysis of the gabapentin.

Digital Childhood: the Impact of Using Digital Technology on Children’s Health

Background and Objective: Digital media can be considered as an important element of life for today's children and adolescents since theyspend a lot of time using it. This increased use of digital media is associated with poor behavior and health status. Society in general andpractitioners in public health in particular should promote digital media use strategies through health education. This study is aimed atevaluating the impact of using digital technology on children physical, social and behavior health. Methodology: This is a descriptive studywhich was conducted at the primary health care centers of Tabuk. Through purposive sampling, 300 people were included in the study. Aquestionnaire and a checklist were used as the tools for data collection. Results: There was a significant relationship between theattachment to technology and both physical and psychological health of the studied children. There was also a significant differencebetween the awareness of mothers regarding both negative and positive effects of technology and total effects of technology at the pre andpost-intervention stages. Conclusion: Using technology had an impact on both physical and psychological health of children, and there wasan improvement in mothers’ awareness in this regard. This reflects the key role of health education on improving the awareness of mothersabout the effects of using technology on the health of their children.

UV-Visible Chemometrics Approach for the Determination of Selected Adulterants in Claimed Premixed Coffee

@#Introduction: Adulterated premixed coffees have turned into an issue in Malaysia lately and have caught the eye of the authorities due to death reports linked to these products. The major cause of this issue is reported that these premixed coffees have passed food inspection test and eventually released to the market for public consumption. These coffees were claimed to be spiked with several sexual enhancers like sildenafil, tadalafil, and vardenafill, which are common drugs used to treat erectile dysfunction. Methods: Chemometrics approach using UV-Vis spectroscopy was developed to detect the selected sexual enhancer drugs found in commercial coffees by employing SIMCA-P software for the multivariate statistical analysis. Seven brands of coffee samples were purchased from local stores, and 30 sachets each were tested, hence totalling to 210 samples. Each sample was named H, J, G, W, N, T, and K, respectively. Results: Three multivariate models were generated, namely principal component analysis (PCA), orthogonal partial least squares discriminant analysis (OPLS-DA), and partial least squares discriminant analysis (PLSDA). OPLS-DA was selected as the best model for the overall results as it displayed minimal discriminate. Sildenafil, tadalafil, and vardenafil were detected in sample H, while vardenafil in brand J, and none in samples G, W, N, T, and K. Conclusion: OPLS-DA analysis showed discrimination for the sexual enhancer drugs in two brands of premixed coffee. The UV-Vis spectroscopy-based chemometrics method proved to be reliable and efficient in determining the selected drugs, as well as in saving time and cost.

Estructura química de compuestos fenólicos del extracto etanólico de hojas de Clinopodium pulchellum (Kunth) Govaerts "panisara" / Chemical structure of phenolic compounds of the ethanolic extract of leaves of Clinopodium pulchellum (Kunth) Govaerts "Panisara"

Objetivos: Proponer la estructura química de componentes fenólicos aislados del extracto etanólico de hojas de Satureja pulchella "panisara", quien en la actualidad presenta el nombre de Clinopodium pulchellum (Kunth) Govaerts y evaluar preliminarmente el posible efecto antioxidante de los compuestos fenólicos. Materiales y métodos: Se realizó una identificación fitoquímica mediante ensayos de solubilidad, tamizaje fitoquímico, cromatografía en capa fina y espectroscopía UV/VIS. Por otro lado, se realizó un ensayo preliminar de la actividad antioxidante usando la prueba de 1,1-difenil-2-picrilhidracilo (DPPH). Resultados: Se determinó que el extracto etanólico de hojas de Clinopodium pulchellum (Kunth) Govaerts "panisara" es soluble en solventes polares. Los metabolitos secundarios encontrados son compuestos fenólicos tipo flavonoides, alcaloides, quinonas y glicosidos. Se propone siete estructuras químicas de flavonoides a través del análisis de los espectros UV/Vis, y mediante comparación con lo publicado por TJ Mabry y Olga Lock. Al realizar el ensayo preliminar de la actividad antioxidante usando la prueba de 1,1-difenil-2-picrilhidracilo (DPPH) se observó disminución de absorbancia, al aplicar el extracto frente al control. Conclusiones: Se propone la estructura química de 7 metabolitos secundarios tipo flavonas que podrían explicar una posible acción antioxidante del extracto etanólico de hojas de Clinopodium pulchellum (Kunth) Govaerts "panisara".

Caracterización de compuestos fenólicos presentes en el extracto etanólico de hojas de Alternanthera lanceolata (Benth) Schinz, "lancetilla" / Characterization of phenolic compounds present in the ethanolic extract of leaves of Alternanthera lanceolata (Benth.) Schinz, "lancetilla"

Objetivos: Caracterizar compuestos fenólicos presentes en el extracto etanólico de las hojas de Alternanthera lanceolata (Benth.) Schinz "lancetilla". Materiales y métodos: Se preparó un extracto etanólico de las hojas de Alternanthera lanceolata (Benth.) Schinz "lancetilla". Se evaluó la solubilidad del extracto en solventes de polaridad creciente. Se detectaron los componentes químicos del extracto etanólico mediante un tamizaje fitoquímico empleando gelatina, tricloruro férrico, reacción de Shinoda, entre otros. Se realizó cromatografía en capa fina, desorción y propuesta de estructuras químicas para los metabolitos tipo flavonoides presentes en el extracto etanólico de hojas de Alternanthera lanceolata (Benth.) Schinz "lancetilla" mediante espectroscopía UV-Vis. Resultados: El extracto etanólico presentó mejor solubilidad en solventes de mediana polaridad. El tamizaje fitoquímico dio resultados positivos para presencia de compuestos fenólicos, flavonoides y glicósidos. Se propuso la estructura química de siete flavonas en el extracto investigado. Conclusiones: Se caracterizó y propuso las estructuras de compuestos fenólicos tipo flavonas en el extracto etanólico de las hojas de Alternanthera lanceolata (Benth.) Schinz "lancetilla".

Determinacion estructural de flavonoides en el extracto etanolico de cladodios de Opuntia ficus-indica (L.) Mill. "Tuna Verde" / Structural identification of flavonoids in ethanolic extract of Opuntia ficus-indica (L.) Mill. "Tuna Verde" cladodes

Objetivos: Determinar estructuralmente los flavonoides encontrados en el extracto etanólico de cladodios de Opuntia ficus-indica (L.) Mill. "Tuna Verde". Materiales y métodos: Se preparó el extracto etanólico de cladodios de Opuntia ficus-indica (L.) Mill. Luego se detectaron sus componentes mediante un tamizaje fitoquímico. A través de cromatografía en capa fina se aislaron los compuestos fenólicos tipo flavonoides. Finalmente, usando espectroscopia UV/Vis se propuso la posible estructura de los flavonoides encontrados. Resultados: El tamizaje fitoquímico mostró presencia de compuestos fenólicos, flavonoides y glicósidos. Se propuso cinco estructuras químicas de compuestos fenólicos, todas con un núcleo en común: flavona, mediante las lecturas en el espectrofotómetro UV/Vis y por comparación con lo publicado por TJ Mabry. Conclusión: Se determinó la posible estructura química de cinco flavonoides presentes en el extracto etanólico de cladodios de Opuntia ficus-indica (L.) Mill. "Tuna Verde".

Comparison of development methods based on UV/VIS spectrophotometry and ICP OES for the determination of iodine in pharmaceuticals.

In this study, methods based on UV-Vis spectrophotometry (Sandell-Kolthoff reaction) and inductively coupled plasma optical emission spectrometry (ICP OES) were developed in order to determine iodine in pharmaceuticals. A simple preparation of samples, which consisted in the solubilization by means of ultrasound, was performed using pure water as solvent. The developed analytical methods were validated employing limit of detection, precision and accuracy. The recovery range is 101.0% - 104.0% for the expectorant solutions, and 98.0% - 102.0% for the supplements using the ICP OES technique. For the UV-Vis spectrophotometric method, the recovery range is 96.0% - 98.0% for the expectorant solutions, and 96.0% - 98.3% for the supplements. These methods are simple and accessible, and might be used in the pharmaceutical field.

UV-Vis and UPLC fingerprint analysis on various medicinal parts of Gentiana rhodantha and resource evaluation / 中草药

Objective: To develope a method for UV-Vis and UPLC fingerprint on various medicinal parts of Gentiana rhodantha. The chemical compounds variation in roots, steams, leaves, and flowers were studied by using fingerprint data combined with multivariate analysis. Methods: Using Shim-pack XR-ODS III liquid chromatographic column (150 mm × 2.0 mm, 2.2 μm) for gradient elution, mobile phase was water with 0.1% formic acid and acetonitrile, temperature was 40℃, detection wavelength was 242 nm, injection value was 0.3 μL, and flow rate was 1.00 mL/min. Electrospray ionization (ESI) source and MRM model, the interface voltage was set to 3.5 kV. Desolation line (DL) temperature was 250℃. Nebulizing gas and drying gas were nitrogen at a flow rate of 3.0 and 15.0 L/min, respectively. Collision gas was 0.15 mL/min. UV-Vis detection wavelength range at 200 - 500 nm, slit was 1.0 nm, step was 0.5 nm. Multivariate analysis methods including partial least squares discriminant analysis (PLS-DA), variable importance (VIP), and hierarchical cluster were used for this projection. Results: The investigation of UPLC and UV-Vis showed RSD was lower than 2.00% for precision, repeatability, and stability. The recoveries of loganin acid, mangiferin, and sweroside were 97.89% - 102.71% and RSD was 1.09% - 2.88%. Pretreatment by 11 smooth + first order was the best data processing method for PLS-DA model (R2cal = 0.9315, RMSEE = 0.302, R2val = 0.901, and RMSEP = 0.341). UV-Vis spectra of roots, steams, leaves, and flowers had the significant fingerprint characteristic. Similarity analysis showed the chemical compounds in the leaves and flowers were similar and those in the stems and roots were similar too. Similarity index of root medicinal material has a widely range. The quality of the roots was not stable. The contents of loganic acid and mangiferin were the highest in the leaves and flowers [(1.46 ± 0.42) and (51.59 ± 15.45) mg/g]. The content of sweroside was the hightest in the roots [(4.41 ± 3.24) mg/g]. The total content of compounds of the leaves was higher than other medicinal part, the three compounds, loganic acid, mangiferin, and sweroside were very used for the discrimination of different parts of G. rhodantha. Cluster anslysis showed there were geography characteristics of the constituents. Sample collected from high altitude was higher than samples collected from lower altitude. And they were classified in different groups. Conclusion: UPLC and UV-Vis fingerprint could describe the variation of chemical compounds in the roots, steams, leaves, and flowers. All the results could provide the evaluation method and basic theory of G. rhodantha resource.