GC-FID guided Identification and Quantification of detectable Phytochemicals in selected Commercial Chamomile Herbal Tea

Background and objective: Phytochemicals are plant-based bioactive ingredients found in tea, fruits, and vegetables with multiple health benefits. This study aimed to identify and quantify the detectable phytochemicals in selected products of chamomile herbal tea (CHT) using the Gas Chromatography - Flame Ionization Detector (GC-FID) approach. Methods: Selected CHTs were coded as CHT-A to CHT-G. CHT-F was crude and unbranded however, CHT-G was an oil extract of CHT. Ethanolic extracts of CHT were analysed and quantified for their phytoconstituents using the GC-FID method. Results: Phytochemicals detected in their order of abundance in most CHTs were flavonoids > glycosides > alkaloids > steroids > anti-nutrients > saponins > tannins > resveratrol. The flavonoids comprised rutin > flavanone > flavone > anthocyanin > epicatechin > kaempferol > naringenin > proanthocyanin, etc. where the glycosides found in each CHT involved cardiac and cyanogenic glycosides. Alkaloids were highest in CHT-A as ribalinidine > spartein > lunamarin with ephedrine detected just in CHT-B, CHT-C, CHT-D, CHT-E and CHT-F. Saponins occurred in four samples mainly as sapogenin. Anti-nutrients were detected in each CHT and included the phytates and oxalates. Resveratrol was detected in three samples only. Conclusion: Most of the CHTs evaluated showed the presence of flavonoids, glycosides, alkaloids, steroids, anti-nutrients, saponins, tannins and resveratrol.

Extraction and Characterisation of Flavoured Tobacco by GC-MS Studies and Validation of Results by GC-FID to Investigate Hazardous Flavour Ingredients

Flavoured tobacco is mainly consumed in India and neighbouring countries like Pakistan, Afghanistan, and Nepal and the hazards are known. Considering the need to identify such flavouring ingredients and a simple analytical method was required to quantify such favouring ingredients and hazardous / allergens, we selected top brands available in India for investigation. We simply extracted the ingredients by triturating with Diethyl Ether, evaporating solvent ether and reconstituting the extract in Acetone & Ethanol for GC-MS & GC-FID work respectively. The flavour ingredients were identified, and hazardous ingredients, viz. Diethyl Phthalate was identified. It was found around 2.5% to 3.0%. The GC-MS method was validated with GC-FID analysis with Linearity, LOD & LOQ study.

A simple method for the determination of bioethanol from lignocellulosic materials using gas chromatography-flame ionisation detector (GC-FID)

Aims@#The utilisation of lignocellulosic biomass for bioethanol production reduces the dependency on fossil fuels as a source of energy and emission of greenhouse gas (GHG). However, studies in this emerging field are hampered by the cost of ethanol quantification methods. Due to the volatile nature of ethanol, the method for the quantification of bioethanol production should be reproducible and rapid to avoid any evaporation loss to the surroundings. Therefore, this study aimed to develop a simple, rapid and precise bioethanol quantification method using a gas chromatographyflame ionisation detector (GC-FID) without having to go through distillation process for ethanol purification.@*Methodology and results@#The bioethanol was produced via consolidated bioprocessing (CBP) using Trichoderma asperellum B1581 and paddy straw. The peak corresponding to ethanol was obtained at 2.347 min with a peak area of 189.66, equating to 0.159% (v/v) or 1.25 g/L ethanol. A comparison between the quantity of ethanol detected by GC-FID and spectrophotometric analysis (340 nm) showed no significant difference (p>0.05) in the amount of ethanol detected by GC analysis, thus validating the accuracy of the GC method.@*Conclusion, significance and impact of study@#This work presents a simple, precise and reliable method to determine the amount of bioethanol in the sample using a GC-FID. Currently, there are many GC-FID methods available for the determination of ethanol/alcohol in a human blood samples or in beverages but not in bioethanol samples. Thus, this method was developed to facilitate the determination of bioethanol in the samples produced from lignocellulosic materials.

Development of a rapid GC-FID method to simultaneously determine triethylamine,diisopropylamine,and 1,1,3,3-tetramethylguanidine residues in an active pharmaceutical ingredient / 药物分析学报

A rapid GC-FID method was developed to simultaneously determine residual levels of triethylamine(TEA),1,1,3,3-tetramethylguanidine(TMG),and diisopropylamine(DIPA)in the synthetic route of an active pharmaceutical ingredient(API).Due to the severe absorption of amines on GC stationary phases,GC columns with various stationary phases were evaluated for optimal peak shape and reproducibility.The final conditions used the Agilent CP-Volamine column to resolve the three amines in 12 min.Various inlet liners were also screened to further improve the sensitivity of the analysis.The Restek Siltek? liner was selected to achieve the desired detectability for the method.The quantitation limits were 4,3,and 4 μg/mL for TEA,DIPA,and TMG in the presence of API,respectively.All three amines showed good linearity(r＞0.999)and recoveries(＞90％)over the concentration range of 3 to 16 μg/mL.The testing of residual amines was initially performed at the penultimate stage of the synthesis.However,this work demonstrates that TMG can act as a proton sponge to react with salicylic acid,the counter ion of the penultimate,to form a volatile component that elutes at a different retention time.Consequently,in the final method,these three amines were monitored in the final API to circumvent the matrix interference.Key parameters of the method were qualified per method validation requirements in ICH guidelines.The method was successfully applied for batch testing during development and implemented as an in-process control procedure at manufacturing sites.

Fatty acid quantification method by isobutyl esterification and GC-FID/MS / 上海交通大学学报（医学版）

Objective:To establish a quantification method for understanding the varieties and concentrational changes of fatty acids under physiological and pathophysiological conditions. Methods:Based on isobutyl esterification using (-)-menthyl chloroformate and isobutanol, 27 typical fatty acids were qualitatively and quantitatively analyzed by gas chromatography-flame ionization detector/mass spectrometry (GC-FID/MS). The sensitivity and stability of the method were detected by limit of detection (LOD), limit of quantification (LOQ), and intra-day and inter-day relative standard deviation (RSD). The method was applied to four typical biological samples (human serum, urine, feces and rat liver) to verify the universality in different substrates. Results:Isobutyl esters of 27 fatty acids were effectively separated with an HP-5MS column. The results showed nice linearity within 2-3 orders of magnitude in terms of concentration with R2>0.99 for all 27 tested fatty acids. The LODs of the method were between 0.03 and 2.96 pmol on column whereas the LOQs were between 0.09 and 9.86 pmol. The results of method validation showed that the intra-day and inter-day RSDs were all under 10% in the range of high, medium and low concentrations. With this method, moreover, 10, 7, 14 and 9 fatty acids were detected in human serum, urine, feces and rat liver, respectively. Conclusion:A quantitative analytical method for fatty acids with short, media and long chains (C1-C24) is established based on isobutyl estrification in aqueous media. This method has the advantages of mild condition, high sensitivity, good stability, and simple and quick operation, and can be directly used in the detection of serum, urine, feces, liver and other biological samples, which may provide a new idea for high-throughput metabolome analysis.

Phytochemical analysis of Juglans regia oil and kernel exploring their antinociceptive and anti-inflammatory potentials utilizing combined bio-guided GC-FID, GC-MS and HPLC analyses

ABSTRACT Juglans regia L., Juglandaceae, is broadly used due to its immunomodulatory effects, potentials in protecting against many sever-disorders, and high safety-profile. The aim of this work is to make a phytochemical analysis of J. regia oil and kernel exploring their antinociceptive and anti-inflammatory potentials utilizing combined bio-guided gas chromatography with mass spectrometer (GC-MS), gas chromatography with flame ionization detection (GC-FID) and reversed-phase high-performance liquid chromatography (RP-HPLC) analyses. Combined bio-guided GC-MS, GC-FID and RP-HPLC analyses is an innovative-combined-technique aiming at efficiently analyzing various-extracts phytochemical and biological characters. The J. regia oil and kernel ethyl-acetate extract were monitored during exploring their possible acute-antinflammatory, antidiabetic and antidiabetic-neuropathy. Glycated-hemoglobin, serum-insulin, serum-catalase and lipid-peroxidation levels have been also monitored. Combined bio-guided GC-FID, GC-MS and HPLC analyses have shown to be an efficient analyzing-method through identifying the most active compound, linoleic acid. Linoleic acid has shown the highest improvement of the acute inflammatory-pain, chronic blood-glucose level reduction, serum-insulin elevation, and normalization of glycated-hemoglobin levels. J. regia oil has shown more lipid-peroxidation reduction, while kernel ethyl-acetate extract has shown more acute-blood-glucose level reduction and serum-catalase levels elevation. Compared to tramadol, the highest-doses of J. regia oil, kernel ethyl-acetate extract, and linoleic acid have shown higher antinociceptive-potentials in amelioration of thermal-hyperalgesic and anti-allodynic neuropathic-pain. Thus, the antinflammatory, the reduction of oxidative-stress, and the insulin-secretagogue potentials might be among the possible mechanisms of improvement of neuropathic-pain. In correlation to conventional-techniques, the combined bio-guided analyses have shown to be an efficient innovative-combined technique. After further clinical studies, J. regia might be utilized as a possible-remedy for various painful-syndromes.

Investigation of Ultrasound-assisted Extraction of Pogostemon cablin (Blanco) Benth and Its GC-FID Determination / 世界科学技术-中医药现代化

Objective: To investigate the ultrasound-assisted extraction process of Pogostemon cablin. Methods: Taking the extraction time (min), ethanol concentration (％), and liquid-solid ratio (mL · g-1) as influence factors, patchouli alcohol (PA) content as index, single-factor test was applied to the investigation of extraction-process of Pogostemon cablin. By ultrasonic-assisted extraction, the GC-FID was used to determine the PA content in extract. Results: The optimal extraction conditions were as follows: the ultrasonic time was 30 min, the ethanol concentration was 95％, and liquid-solid ratio was 20∶1 mL·g-1. Under this condition, the extraction rate and the content of PA were 32.75％, and0.15％ respectively. Conclusion: This extraction method is simple, but has higher extraction rate. It is suitable for the industrial production.

Simultaneous determination of four constituents in Kaihoujian Spray by GC-FID / 中成药

AIM To establish a gas chromatography-flame ionization detector (GC-FID) method for the simultaneous content determination of four constituents in Kaihoujian Spray (a spray for management of oral and laryngopharyngeal inflammatory condition,containing Sophorae tonkinensis Radix et Rhizoma,Cicadae Periostracum,menthol,etc.).METHODS The analysis of mixure of Kaihoujian Spray and internal standard (dibutyl phthalate) solution was conducted on an HP-INNOWax column (30 m ×0.25 mm ×0.25 μm),both of the injector temperature and detector temperature were set at 260 ℃,the split ratio was 5 ∶ 1,and the flowing rate was 1.5 mL/min.RESULTS Menthol,matrine,sophocarpine and sophoridine showed good linear relationships within the ranges of 0.228 7-2.287 0 mg/mL (r =0.999 7),0.011 1-0.111 0 mg/mL (r =0.999 6),0.016 8-0.168 0 mg/mL (r =0.999 8) and 0.003 4-0.034 0 mg/mL (r =0.999 4),whose average recoveries (n =9) were 98.4％ (RSD=1.2％),95.9％ (RSD=1.8％),96.2％ (RSD=2.1％) and 97.1％ (RSD=1.7％),respectively.CONCLUSION This accurate,sensitive and simple method can be used for the quality control of Kaihoujian Spray.

Analytical method validation of GC-FID for the simultaneous measurement of hydrocarbons (C2-C4) in their gas mixture / Validación de un método analítico GC-FID para la medida simultánea de hidrocarburos (C2-C4) en una mezcla gaseosa / Validação de uma metodologia analítica GC-FID para a medida simultánea de hidrocarbonetos (C2-C4) em uma mistura gasosa

An accurate gas chromatography coupled to a flame ionization detector (GC-FID) method was validated for the simultaneous analysis of light hydrocarbons (C2-C4) in their gas mixture. The validation parameters were evaluated based on the ISO/TEC 17025 definition including method selectivity, repeatability, accuracy, linearity, limit of detection (LOD), limit of quantitation (LOQ), and ruggedness. Under the optimum analytical conditions, the analysis of a gas mixture revealed that each target component was well-separated with high selectivity property. The method was also found to be precise and accurate. The method linearity was found to be high with good correlation coefficient values (R² ≥ 0.999) for all target components. It can be concluded that the GC-FID developed method is reliable and suitable for determination of light C2-C4 hydrocarbons in their gas mixture. The validated method was successfully applied to the estimation of light C2-C4 hydrocarbons in natural gas samples, showing high performance repeatability with relative standard deviation (RSD) less than 1.0% and good selectivity with no interference from other possible components.

Se validó una cromatrografía de gases precisa, acoplada con un detector de ionización de llama (GC-FID) para el análisis simultáneo de hidrocarburos ligeros (C2-C4) en su mezcla gaseosa. Los parámetros de validación se evaluaron con base en la definición de la ISO/ IEC 17025, que incluye selectividad del método, precisión y repetibilidad, exactitud, linealidad, limite de detección (LOD), limite de cuantificación (LOQ) y robustez. Bajo las condiciones analiticas óptimas, el análisis de la mezcla gaseosa mostró que cada analito de interés fue separado adecuadamente con alta selectividad. Se encontró también que el método fue preciso y exacto; la linealidad fue alta y con buen coeficiente de correlación lineal (R² ≥ 0.999) para todos los analitos. Se puede concluir que el método GC-FID es confiable y apropiado para la determinación de hidrocarburos ligeros C2-C 4 en una mezcla gaseosa. El método validado ha sido exitosamente aplicado a la valoración de hidrocarburos ligeros C2-C4 en muestras de gas natural, mostrando alta repetibilidad con desviación estándar relativa (RDS) menor al 1% y buena selectividad sin interferencias de otros posibles componentes.

Foi avaliada uma cromatografia gasosa precisa, equipada com um detector de ionização de chama (CG-FID) para a análise simultâneo de hidrocarbonetos ligeiros (C2-C4) em uma mistura gasosa. Os parâmetros de validação foram avaliados baseados na definição da ISO/IEC 17025, que inclui seletividade do método, precisão e repetibilidade, exatidão, linearidade, limite de detecção (LOD), limite de quantificação (LOQ) e robustez. Baixo as condições analiticas ótimas, a análise da mistura gasosa mostrou que cada analito foi separado adequadamente com alta seletividade. Também foi encontrado que o método foi preciso e exato; a linearidade foi alta e com bom coeficiente de correlação linear (R² ≥0.999) para todos os analitos. Pode-se concluir que o método GC-FID é confiável e apropriado para a determinação de hidrocarbonetos ligeiros C2-C4 em uma mistura gasosa. O método avaliado têm sido exitosamente aplicado à valoração de hidrocarbonetos ligeiros C2-C4 em amostras de gás natural mostrando alta repetibilidade com desvio-padrão relativo menor funcionais. ao 1% e boa seletividade sem interferências de outros possiveis componentes.

Chemical monitoring of canola, corn, olive, soybean and sunflower oils after thermal treatment at conventional temperatures in domestic stoves / Monitoramento químico de óleos de canola, milho, azeitona, soja e girassol após tratamento térmico a temperaturas convencionais em fogões domésticos

The frying by immersion is a widely used cooking process and it improves the food texture and flavor. This study analyzed the initial thermal oxidation in five edible vegetable oils used forfrying. Oils samples were heated twice for 30 minutes, at 180 °C and then at 240 °C simulating the domestic stoves temperatures. The oils decomposition temperatures were determined byTG, being all of them > 250 °C. The FA profile was analyzed by GC-FID and a slight decrease of UFA was found in corn and soybean oils. In canola, olive and sunflower oils, UFA was stableafter heating treatment. Minor FA decomposition was found in canola oil, and followed by corn, olive, sunflower and soybean oils. NIR spectroscopy analyzes resulted in an extensive bands overlapping. The spectra were modeled by PCA and the oils were classified into two groups: fresh oil and heated oil, mainly by differing in 1900 nm region, associated with the carboxyl signal decrease, which might be related to the initial FA degradation in samples. It could partiallyunderstand what occurs to the vegetable oil in the beginning of its thermo-decomposition. These information are useful to consumers, food industry and health surveillance agency.

A fritura por imersão é um processo de cozimento amplamente utilizado e melhora a textura e o sabor do alimento. Este estudo analisou a oxidação térmica inicial em cinco óleos vegetais comestíveis usados ​​para fritar. As amostras de óleo foram aquecidas duas vezes durante 30 minutos, a 180 ° C e depois a 240 ° C simulando as temperaturas dos fogões domésticos. As temperaturas de decomposição dos óleos foram determinadas por TG, sendo todas elas> 250 ° C. O perfil de FA foi analisado por GC-FID e uma ligeira diminuição de UFA foi encontrada em óleos de milho e de soja. Nos óleos de canola, azeite e girassol, a UFA foi estável após o tratamento térmico. A decomposição menor de FA foi encontrada em óleo de canola, seguido de óleo de milho, azeite, girassol e soja. As análises de espectroscopia NIR resultaram em uma ampla faixa de sobreposição. Os espectros foram modelados por PCA e os óleos foram classificados em dois grupos: óleo fresco e óleo aquecido, principalmente por diferença na região de 1900 nm, associado à diminuição do sinal carboxílico, o que pode estar relacionado à degradação inicial de FA nas amostras. Poderia entender parcialmente o que ocorre ao óleo vegetal no início de sua termo-decomposição. Essas informações são úteis para consumidores, indústria de alimentos e agência de vigilância da saúde.

Chemical monitoring of canola, corn, olive, soybean and sunflower oils after thermal treatment at conventional temperatures in domestic stoves / Monitoramento químico dos óleos de canola, milho, oliva, soja e girassol após tratamento térmico em temperaturas alcançadas por fogões domésticos

The frying by immersion is a widely used cooking process and it improves the food texture and flavor. This study analyzed the initial thermal oxidation in five edible vegetable oils used for frying. Oils samples were heated twice for 30 minutes, at 180 C and then at 240 C simulating the domestic stoves temperatures. The oils decomposition temperatures were determined by TG, being all of them > 250 C. The FA profile was analyzed by GC-FID and a slight decrease of UFA was found in corn and soybean oils. In canola, olive and sunflower oils, UFA was stable after heating treatment. Minor FA decomposition was found in canola oil, and followed by corn, olive, sunflower and soybean oils. NIR spectroscopy analyzes resulted in an extensive bands overlapping. The spectra were modeled by PCA and the oils were classified into two groups: fresh oil and heated oil, mainly by differing in 1900 nm region, associated with the carboxyl signal decrease, which might be related to the initial FA degradation in samples. It could partially understand what occurs to the vegetable oil in the beginning of its thermo-decomposition. These information are useful to consumers, food industry and health surveillance agency.

A fritura por imersão é um processo de cocção utilizado pela inclusão de textura e sabor aos alimentos. Foi analisada a oxidação térmica inicial de cinco óleos vegetais comestíveis utilizados para fritura de imersão. Amostras de óleos foram aquecidas duas vezes por 30 minutos, a 180 ºC e depois a 240 ºC, simulando-se as temperaturas de fogões domésticos. As temperaturas de decomposição dos óleos foram determinadas por TG, sendo > 250 ºC. O perfil de FA foi analisado por GC-FID, detectando-se pequeno decréscimo dos UFA nos óleos de milho e soja. Nos óleos de canola, oliva e girassol, os UFA foram estáveis após o tratamento térmico. A menor decomposição dos FA foi detectado no óleo de canola, seguido de milho, oliva, soja e girassol. Análises por espectroscopia NIR resultaram em grande sobreposição das bandas. Os espectros foram modelados por PCA, classificando-se os óleos em dois grupos: óleo fresco e óleo aquecido, principalmente pelas diferenças na região de 1900 nm, relacionadas ao decréscimo do sinal de carboxilas, e associadas à degradação inicial dos FA nas amostras. Ainda que parcialmente, pode-se entender o que ocorre com os óleos vegetais no início de termo-decomposição, abrangências que são úteis para consumidores, indústria alimentícia e órgão de vigilância sanitária.

Composition of the essential oil from leaves of Smallanthus quichensis (Asteraceae) from Costa Rica / Composición química del aceite esencial de las hojas de Smallanthus quichensis (Asteraceae) de Costa Rica

Smallanthus is a genus of flowering plants in the Asteraceae family, which has about 24 species, ranging mostly from southern Mexico and Central America to the Andes in South America. The aim of the present study was to identify the chemical composition of leaf essential oil of S. quichensis, growing wild in Costa Rica. The extraction of the oils was carried out by the hydrodistillation method, using a modified Clevenger type apparatus. The chemical composition of the oils was analyzed by capillary GC-FID and GC-MS using the retention indices on DB-5 type capillary column. A total of 100 compounds were identified, accounting for about 90 percent of the total amount of the oils. Smallanthus quichensis leaf produced a monoterpenoid-rich oil, whose composition was dominated by αlfa-pinene (64.5 percent) and 1,8-cineole (9.7 percent) or, in a different sample, by αlfa-pinene (35.5 percent) with moderate amounts of p-cymene (11.5 percent), beta-phellandrene (9.2 percent), alfa-phellandrene (9.0 percent) and limonene (5.8 percent). This is the first report of the chemical composition of the essential oil obtained from this plant species.

Smallanthus es un género de plantas perteneciente a la familia Asteraceae que contiene aproximadamente 24 especies, la mayoría ubicadas desde el sur de México, América Central y hasta la cordillera de los Andes en América del Sur. El objetivo del presente estudio fue el de identificar la composición química del aceite esencial de las hojas de S. quichensis. La extracción se realizó mediante el método de hidrodestilación, empleando un instrumento de tipo Clevenger. Se analizó la composición de los aceites mediante CG-FID y CG-EM, utilizando índices de retención obtenidos en una columna capilar tipo DB-5. Se identificaron 100 compuestos, correspondientes a un 90 por ciento de los constituyentes totales. Los aceites están constituidos principalmente por monoterpenoides (ca. 85 por ciento). Los componentes mayoritarios se identificaron como alfa-pineno (64.5 por ciento), acompañado por 1,8-cineol (9.7 por ciento) o, en otra muestra distinta, αlfa-pineno (35.5 por ciento) junto a cantidades moderadas de p-cimeno (11.5 por ciento), beta-felandreno (9.2 por ciento), alfa-felandreno (9.0 por ciento) y limoneno (5.8 por ciento). Este es el primer informe acerca de la composición química de aceites esenciales obtenidos de S. quichensis.

Análisis de cocaína en diferentes muestras por cromatografía de gases con detector de ionización de llama (CG-FID) / Analysis of cocaine in different samples by gas chromatography flame ionization detector (GC-FID) / Análise de cocaína em diferentes amostras por cromatografia gasosa com detector de ionização de chama (GC-FID)

En este estudio se realizó la validación de los métodos establecidos por la UNODC para la cuantificación y extracción de benzometilecgonina (cocaína) presente en las hojas de Erythhroxylum coca, en té de coca y en clorhidrato de cocaína. El primer método de extracción, recomendado por la UNODC, es una extracción solido-líquido (ESL), sin embargo, los resultados obtenidos indican que esta no es lo suficientemente eficiente para lograr una señal de analito distinguible de la relación señal a ruido (S/N) para las muestras de hojas de Erythhroxylum coca y té de coca. El segundo método propuesto es la extracción soxhlet, los resultados indican que esta resulta más eficiente para aislar y cuantificar el analito de interés por cromatografía de gases acoplada a un detector de ionización por llama (CG-FID). Después de someter las muestras al proceso de extracción soxhlet y cuantificación por CG-FID se encontró que la hoja de té posee 7,66×10² mg de cocaína/kg de muestra, las hojas de coca 17,15 mg de cocaína/kg de muestra y el clorhidrato de cocaína 7,15×10(5) mg de cocaína/kg de muestra. El método de análisis escogido se caracteriza por arrojar bajos límites de detección (0,169 mg/L) y por poseer parámetros estadísticos y cromatográficos ideales.

In this study validate the methods established by the UNODC for quantification and extraction benzometilecgonina (cocaine) in the leaves of Erythhroxylum coca, coca tea and cocaine hydrochloride. The first extraction method recommended by the UNODC is a solid-liquid extraction (ESL), however, the results indicate that this is not efficient enough to achieve analyte signal distinguishable from the signal to noise ratio (S/N) for samples Erythhroxylum coca leaves and coca tea. The second proposed method is soxhlet extraction, the results indicate that this is more efficient to isolate and quantify the analyte of interest by gas chromatography coupled to a flame ionization detector (GC-FID). After submitting the samples to the soxhlet extraction process and quantification by GC-FID it found that tea leaf has 7.66×10² mg of cocaine/kg sample, coca leaves 17.15 mg of cocaine/kg sample and cocaine hydrochloride concentration corresponded to 7.15×10(5) mg of cocaine/kg sample. The chosen analysis method is characterized by low detection limits shed (1.69 mg/L) and possessing ideal chromatographic and statistical parameters.

Neste estudo validaram-se os métodos estabelecidos pelo UNODC para a quantificação e extração de benzometilecgonina (cocaína) nas folhas de Erythhroxylum coca; em chá de coca e cloridrato de cocaína. O primeiro método de extração recomendado por UNODC é uma extração sólido-líquido (ESL), no entanto, os resultados indicam que esta não é suficientemente eficaz para atingir um sinal de analito distinguível da relação sinal-ruído (S/N) para amostras de folhas Erythhroxylum coca e chá de coca. O segundo método proposto é uma extração soxhlet, os resultados indicam que este é mais eficiente para isolar e quantificar o analito de interesse por cromatografia gasosa acoplada a um detector de ionização de chama (GC-FID). Depois de enviar as amostras para o processo de extração soxhlet e quantificação por GC-FID descobriu-se que as folhas de chá têm 7,66×10² mg de cocaína/kg de amostra, as folhas de coca 17,15 mg de cocaína/kg de amostra e o cloridrato de cocaína 7,15×10(5) mg de cocaína/kg de amostra. O método de análise escolhido é caracterizado por ter baixos limites de detecção (1,69 mg/L) e possuir parâmetros estatísticos e cromatográficos ideais.

Clinical Evaluation and Serum Lipid Profile between Individuals with Acute Hepatitis C.

Aim: Hepatitis C virus (HCV) exerts an intense impact on host lipid metabolism. It has been shown that the synthesis of cholesterol and fatty acids (FA) is directly affected in HCV patients but serum FA profile of acute HCV patients have not been directly quantified in humans. Methodology: In present study the serum lipid and FA’s profile (free and total) of acute hepatitis C patients (n=50) is evaluated in comparison to healthy controls (n=50). The acute HCV patient’s were diagnosed by center of diseases control (CDC) criteria. Blood hematology, serum proteins, enzymes, waste metabolites and nutrition status were also assessed by standard methods. Results: The acute HCV patients have significantly lower (P<0.05) lipid profile including triglycerides, cholesterol, HDL and LDL in relation to controls. Results of serum lipid FA’s (total and free form) reveal elevated level of saturated fatty acid (SFA) and monounsaturated fatty acid (MUFA), with lower content of polyunsaturated fatty acid (PUFA) in acute hepatitis C patient as compared to controls. Among SFA, myristic and palmitic acid were increased and five unsaturated FA including nervonic, linoleic, α-linolenic, docosahexaenoic and arachidonic acid were reduced than control subjects. Significantly higher (P<0.05) alanine transaminase, alkaline phosphatase, direct bilirubin and globulin levels were found in acute HCV patients possibly due to viral infection. Conclusion: This work makes available direct proof that lipogenesis is elevated in acute HCV patients while as evident from reduced serum PUFA and elevated SFA as well as MUFA. Hence acute HCV patients have low PUFA levels, which put forward importance of PUFA supplementation.

Desarrollo y validación de un método verde para la extracion y cuantificación de residuos de cipermetrina en tejido animal / Fevelopment and validation of green method for the extraction and quantification of cypermethrin residues in animal tissue / Desenvolvimento e validação do método verde para a extração e quantificação dos resíduos da cipermetrina no tecido animal

En este trabajo se desarrolló y validó un método simple, ambientalmente amigable y efectivo, para la extracción y cuantificación de cipermetrina en muestras de bovino (hígado, grasa perirrenal y músculo) utilizando dispersión de matriz en fase sólida (MSPD) y cromatografía de gases con detector de ionización de llama (GC-FID). Diferentes parámetros del método se evaluaron, tales como el dispersante, solvente de extracción y volumen de solvente. Los mejores resultados para la extracción de cipermetrina por MSPD fueron: 0,20 g de muestra macerados con 0,80 g de silica gel y extraídos con 5,00 mL de acetona. El procedimiento propuesto fue validado mostrando comportamiento lineal en el intervalo de 10,20-400,40 µg/L (R²=0,9988). Los límites de detección y cuantificación fueron 2,00 y 5,70 µg/L respectivamente, con una desviación estándar relativa de 0,0875 (n=5). Este método permite determinar cipermetrina hasta niveles traza en muestras de tejido animal, con una recuperación de 98,96%.

In the present study a simple, effective and environmentally friendly method was developed and validated for the extraction and quantification of cypermethrin in animal tissue (meat, fat and liver) based on matrix solid-phase dispersion (MSPD) and gas chromatography with flame ionization detector (GC-FID). Different parameters of the method were evaluated, such as dispersant, extractive solvent and solvent volume. The best results for the extraction of cypermethrin by MSPD were 0.20 g of sample with 0.80 g of silica gel and 5.00 mL of acetone as eluting solvent. The proposed procedure was validated showing linear behavior in the interval of 10.20 to 400.40 µg/L (R²= 0.9988). Detection and quantification limits ranged from 2.00 and 5.70 µg/L respectively, with a standard deviation of 0.0875 (n=5). This method enables to determine cypermethrin at trace level in animal tissue samples, with a recovery of 98.96%.

Neste trabalho foi desenvolvido e validado um método verde para extração e quantificação de cipermetrina em amostras de fígado, gordura perirrenal e músculo em gado bovino, por meio da técnica de dispersão de matriz em fase solida (MSPD) e cromatografia de gases com detecção de ionização de chama (GC-FID). Foram avaliados diferentes parâmetros do método, como dispersante, extração com solvente e volume de solvente. Os melhores resultados para a extracção da cipermetrina por MSPD foram 0.20 g da amostra macerada com 0.80 g de gel de sílica e extraiu-se com 5.00 mL de acetona. O método proposto foi validada mostrando um comportamento linear na gama testada (10.20-400.40 µg/L) com R² de 0.9988. Os limites de detecção e de quantificação foram 2.00 e 5.70 µg/L, respectivamente, com um desvio padrão de 0.0875 (n = 5). O método proposto neste trabalho permitiu determinar níveis traça da cipermetrina em amostras de tecidos animai, com uma recuperação de 98.96%.

Essential oil composition and isolation of freeradical-scavenging phenolic glycosides from the aerial parts of Ajuga chamaepitys growing in Iran

From the methanolic extract of the aerial parts of Ajuga chamaepitys (L.) Schreb., Lamiaceae, one of the Iranian medicinal plants, the phenylethanoid glycoside, acteoside, and two flavone glycosides, chrysoeriol 7-O-glucopyranoside (3'-methoxy-luteolin 7-O-glucopyranoside) and apigenin 7-O-rhamnopyranoside, were isolated by a combination of solid-phase extraction (SPE) and preparative reversed-phase high-performance liquid chromatography (prep-RP-HPLC) methods. Structures of the isolated compounds were elucidated by spectroscopic means. The free-radical-scavenging properties of the extracts, fractions and isolated compounds were determined by the 2,2-diphenyl-1-picryl-hydrazyl (DPPH) assay. While among the extracts, the MeOH extract showed the highest level of free-radical-scavenging activity (RC50 1.15 × 10-1 mg/mL), chrysoeriol 7-O-glucopyranoside was the most active (RC50 3.00 × 10-3 mg/mL) among the isolated compounds. The GC-MS and the GC-FID analyses revealed α-pinene (23.66%), β-pinene (9.33%), 1-octen-3-ol (9.72%), β-phellandrene (8.70%) and germacrene-D (7.92%) as the major components of the essential oils derived from the aerial parts of this plant. The presence of phenolic glycosides and the α- and β-pinene-rich essential oils in A. chamaepitys may provide some rationale for the traditional medicinal uses of this species in Iran.

Comparação de métodos analíticos para quantificação de ácido valproico / Comparison of analytical methods for determination of valproic acid

As intoxicações por medicamentos são predominantes no Brasil e frequentes na faixa etária de 0 a 14 anos. O ácido valproico (AV) vem se destacando em virtude do aumento do seu espectro de utilização na terapêutica clínica, porém, a hepatotoxicidade pode ser desencadeada por altas concentrações desse fármaco, apresentando alta incidência em crianças. Logo, tornam-se importantes métodos rápidos de quantificação desse fármaco, a fim de auxiliar o clínico no tratamento da intoxicação. Diante desse cenário, os objetivos deste trabalho foram comparar metodologias analíticas para quantificação de AV por CLAE-F (fluorescência) e CG/DIC (detecção por ionização de chama) em relação à sua potencial aplicação em toxicologia clínico-laboratorial de urgência. Para quantificação de AV por fluorescência, realizou-se a derivatização do AV com 4-(Bromometil)-7-metoxicumarina, sendo o produto da reação analisado em λ de emissão de 325 e detecção de 398 nm, na faixa de calibração de 1-300miug/mL. Com relação à CG/DIC, esta apresentou-se linear na faixa de 100-2000 miug/mL, sem necessidade de derivatização prévia. A técnica de CG/DIC mostrou-se mais apropriada para análises toxicológicas de urgência em casos de intoxicação com AV, tendo em vista o menor tempo de corrida, a linearidade obtida, menor custo, rapidez e praticidade, além de utilizar um equipamento robusto, disponível na grande maioria dos laboratórios de toxicologia de pequeno e médio porte.

Poisoning by drugs is rather frequent in Brazil in the age range of 0 to 14 years. Intoxication by valproic acid (VA) stands out because of an increase in its spectrum of clinical use; hepatotoxicity is an important reaction that can be triggered by high concentrations of this drug and there is a high incidence of toxic events in children. Therefore, fast methods of analysing this drug are essential, in order to help the clinician to treat the intoxication. Given this scenario, the objective of this study was to compare analytical methods to determine VA, by HPLC-F (fluorescence) and GC/FID (flame ionization detection), assessing their potential application in the urgent toxicology clinic. For the fluorometric analysis, the VA was first derivatized with 4-bromomethyl-6, 7-dimethoxycoumarin, and the resulting compound was excited at λ = 325 nm and detected by the emission at 398 nm. The calibration range was 1-300 miug/mL. The GC/FID method showed a linear response in the range 100-2000 miug/mL, without requiring prior derivatization. The technique of GC/FID proved more appropriate for the urgent toxicological analysis of VA, in view of the shorter time of analysis, linearity, lower cost, speed, efficiency and the use of robust equipment that is already available in the great majority of small and medium-sized toxicological clinics.

Optimización de método de microextracción en fse sólida acoplada a cromatograafía gaseosa para análisis de metanol nn agua / Optiization of ssolid phase microextaction method coupled to gas chhromatography for analysis of methanol in water / Otmização do méttodo de microextraão em fase sólida acoplada á crromatografia gasosa para análise de metanol em água

Se optimizó la técnica de microextracción en fase sólida acoplada a cromatografía gaseosa con detector de ionización de flama (HS-SPME/GC-FID por su nombre en inglés) para análisis de metanol en agua utilizando diferentes microfibras, una fibra de poliacrilato y una fibra de polidimetilsiloxano y una columna RTX-5. Las variables evaluadas fueron tiempo de absorción del contaminante en la fibra, volumen libre en el vial, tiempo y temperatura de desorción y efecto de la agitación y presencia de sal en el sistema. De acuerdo con los resultados, el tiempo óptimo de absorción es 15 minutos, el volumen de muestra es 5 mL. Se encontró que existe una íntima relación entre la temperatura de desorción y el área del pico cromatográfico, y una correlación R² = 0,99965 para la curva de calibración elaborada en un rango entre 0 y 50%, considerando el origen, con un límite de detección de 0,01% y un límite de cuantificación del 0,04%.

The technique head space-solid phase micro extraction with gaseous chromatography by using flame ionization detector (HS-SPME/GC-FID) for analysis of methanol in water was optimized using different microfibers, a polyacrylate fiber and a polydimethylsiloxane fiber and a RTX-5 column. The evaluated variables were time of absorption of the pollutant on the fiber, free volume in the vial (free space), time and temperature of desorption as well as effect of agitation and presence of salt in the system. According to the results, the optimal absorption time is 15 minutes, the optimal volume of sample is 5 mL. A close relationship between the temperature of desorption and the chromatographic peak area was found, and a correlation R² = 0.99965 was obtained for the calibration curve in a range between 0 and 50%, considering the origin, with a detection limit of 0.01% and a quantification limit of 0.04%.

A técnica microextração em fase sólida acoplada a cromatografia gasosa com detector de ionização de chama (HS-SPME/GC-FID por seu nome em Inglês) foi otimizada para análise de metanol em água através de diferente micro fibra, uma fibra de poliacrilato e uma fibra de polidimetilsiloxano e uma coluna de RTX-5. As variáveis avaliadas foram tempo para absorver o poluente no volume de fibra livre no frasco, tempo e temperatura de dessorção e efeito da agitação e da presença de sal no sistema. De acordo com os resultados, o tempo de absorção ideal é 15 minutos, o volume da amostra é 5 mL. Descobrimos uma íntima relação entre a temperatura de dessorção e área do pico cromatográfico, e uma correlação R2 = 0,99965 para a curva de calibração desenvolvida em uma escala entre 0 e 50%, considerando a origem, com um limite de detecção de 0,01% e um limite de quantificação de 0,04%.

Estandarizacióndde un método analítico para extacción y cuantificación de cipeermetrina en pastos / Standardizatio oof analytical method for extraction and quantiication of cypeermetrhin in grass / Padronização demmétodo analítico para extração e quantificação de cipermetrina em pattagens

En el presente trabajo se estandarizó un método analítico para la extracción y determinación de cipermetrina en muestras de pastos utilizando microextracción en fase sólida (MEFS) en modo de inmersión con posterior desorción y determinación por cromatografía de gases con detector de ionización de llama (CG-DILL). Las condiciones óptimas para la extracción de cipermetrina en pastos por ID-MEFS fueron: 5 g de muestra se calentaron con 10 mL de solución acuosa de acetona al 1% v/v durante 10 minutos; de esta solución se tomaron 4 mL para llevar a cabo el proceso de extracción por MEFS utilizando una fibra de PDMS con exposición de 30 min a 500 rpm y 60 °C. La desorción del analito se llevó a cabo a 270 °C durante 6 minutos. El procedimiento propuesto mostró comportamiento lineal en el rango probado (5-300 µg/L) con R² de 0,999. Los límites de detección y cuantificación fueron 1,53 y 4,97 ng/mL, respectivamente, con una desviación estándar relativa de 8,57% (n = 6). El método propuesto en este trabajo permite determinar cipermetrina en muestras de pastos hasta niveles de trazas con una recuperación de 99,08%.

In this study, an analytical method has been developed to determine cypermethrin in grass matrices using direct immersion solid-phase microextraction (DI-SPME), coupled to gas chromatography with flame ionization detector (GC-FID). The optimized DI-MEFS experimental procedures to extract cypermethrin in grass matrix were: 5 g of the sample were heated with 10 mL of acetone 1% v/v in water during 10 min. 4 mL of this solution were used for extracting with a polydimethylsiloxane (PDMS)-coated fiber at 60 °C and 500 rpm during 30 min. The analyte desorption was performed at 270 °C for 6 min. The proposed procedure showed linear behavior in the range tested (5-300 mg/L) with R² of 0.999. The detection and quantification limits were 1.53 and 4.97 ng/ mL respectively with a standard deviation of 8.57% (n = 6). The method proposed in this paper allows determining cypermethrin in samples of grass to trace levels with a recovery of 99.08%.

No presente estudo, se padronizou um método analítico para a extração e determinação de cipermetrina em amostras de grama usando microextração em fase sólida (MEFS) no modo de imersão com dessorção subseqüentes e determinação por cromatografia gasosa com detector de ionização de chama (CG-DIC). As condições ótimas para a extração de cipermetrina em pastagens por ID-MEFS foram: 5 g de amostra foram aquecidos com 10 mL de solução aquosa de acetona a 1% v/v por 10 minutos. Desta solução, 4 mL foram tomadas para executar o processo de extração MEFS utilizando uma fibra PDMS submetida por 30 min a 500 rpm e 60 °C. A dessorção do analito foi realizada a 270 °C por 6 minutos. O procedimento proposto apresentou um comportamento linear no intervalo testado (500-300 mg/L) com R² de 0,999. Os limites de detecção e quantificação foram 1,53 e 4,97 ng / mL, respectivamente, com um desvio padrão relativo de 8,57% (n = 6). O método proposto neste trabalho possibilita determinar cipermetrina em amostras de pastagens com uma recuperação de 99,08% nos traços.

Chemical constituents of the volatile oil from leaves of Annona coriacea and in vitro antiprotozoal activity

The essential oil of the leaves from Annona coriacea Mart., Annonaceae, was extracted by hydrodistillation in a Clevenger apparatus and analyzed by GC/MS and GC/FID. The oil yield was 0.05 percent m/m. Sixty compounds were identified, in a complex mixture of sesquiterpenes (76.7 percent), monoterpenes (20.0 percent) and other constituents (3.3 percent). Bicyclogermacrene was its major compound (39.8 percent) followed by other sesquiterpenes. Most of the monoterpenes were in low concentration (<1 percent). Only β-pinene and pseudolimonene presented the highest level of 1.6 percent. The volatile oil presented anti-leishmanial and trypanocidal activity against promastigotes of four species of Leishmania and trypomastigotes of Trypanosoma cruzi, showing to be more active against Leishmania (L.) chagasi (IC50 39.93 µ g/mL) (95 percent CI 28.00-56.95 µ g/mL).