Chemical Characterization and Antiradical Properties of Pyroligneous Acid from a Preserved Bamboo, Guadua angustifolia Kunth

Abstract Pyroligneous acid (PA) was obtained by condensation of the vapors produced in the thermal decomposition of culms residues from Guadua angustifolia Kunth (G. angustifolia) cultivated in Colombia, with and without previous preservation treatment with borax salts. Chemical characterization by GC-MS showed that PA extracts has high content of phenolic compounds. Mequinol, isocreosol, 4-ethylphenol, 4-ethyl-2-methoxyphenol, 3,5-dimethoxy-4-hydroxytoluene and 2,6-dimethoxyphenol were the most abundant substances, identified. The total phenolic content (TPC) and DPPH free radical scavenging activity, were investigated. TPC showed a concentration of 1.959 mg GA g-1±0.010 and 3.844 mg GA g-1±0.027 to PAC and PAS samples. These samples also exhibited high DPPH activity of 70.975%±0.921 and, 16.667%±0.298, respectively. The chemical composition, TPC and DPPH results indicate that the PA extracts obtained from G. angustifolia may be used as a raw material in the food industry as natural preservative, in medicine as alternative to antibiotics and in agriculture as insect repellent and foliar fertilizer.

Validación de un método para cuantificar ácido-11-nor-9-carboxi-delta 9-tetrahidrocannabinol en orina por cromatografía gaseosa-espectrometría de masas previa extracción en fase sólida / Validation of a method for quantify 11-nor-9-carboxy-delta 9-tetrahydrocannabinol in human urine using solid phase extraction and gas chromatography-mass spectrometry

El cannabis es una de las drogas ilegales más usadas a nivel mundial. Su consumo se relaciona con diferentes hechos en el ámbito forense, laboral, deportivo y clínico. Para su detección se utilizan métodos con diferentes fundamentos y alcances (inmunológicos, cromatográficos). En este trabajo se describe un método preciso, reproducible y validado, para la cuantificación del principal metabolito urinario del Δ9-tetrahidrocannabinol, el ácido-11-nor-9-carboxi- Δ 9-tetrahidrocannabinol (THC-COOH), por cromatografía gaseosa-espectrometría de masas (GC-MS). Se efectuó una extracción en fase sólida (SPE) a partir de la orina, previa hidrólisis alcalina. Se utilizó el análogo deuterado (THC-COOH D3) como estándar interno. El análisis por GC-MS se realizó en modo SIM. La curva de calibración fue lineal en el rango de trabajo (10-100 ng/ml, r > 0,999) y el límite de cuantificación fue de 10 ng/ml. La recuperación absoluta estuvo comprendida entre el 91,0 y 99,0 %. La precisión intra e inter ensayo fue de 1,06 a 1,26 y 3,59 a 9,80 %, respectivamente. El método fue aplicado a muestras reales, positivas por test inmunológico, resultando ser muy útil y fiable en el análisis de rutina de THC-COOH en orina humana con fines toxicológicos.

Cannabis is one of the most widely used illegal drug in the world. Its consumption is related to different forensic, work, sports and clinical events. In order to determinate the presence of cannabis, different methods with distinct fundamentals and scopes (immunoassay and chromatography) are applied. This report described an accurate, reproducible, and validated gas chromatography-mass spectrometry (GC-MS) method for the quantitation of 11-nor-9-carboxy- Δ9-tetrahydrocannabinol (THCCOOH), the major metabolite of Δ9-tetrahydrocannabinol in urine. A solid phase extraction (SPE), previous alkaline hydrolysis, was performed on the urine sample. Its deuterated analog (THC-COOH D3) was used as internal standard. The GC-MS analysis made by selected ion monitoring (SIM). Calibration curve was linear over the specified range (10 -100 ng/ml; r > 0.999) and limit of quantitation was 10 ng/ml. Absolute recoveries ranged from 91.0 to 99.0. Intra-assay and inter assay precision ranged from 1.06 to 1.26 and 3.59 to 9.80 %, respectively. The method has been applied to real samples, positive to immunological screening test, resulting to be very useful and reliable in routine analysis of THC-COOH in human urine for toxicological purposes.

Screening analysis of 4 710 cases of inherited metabolic diseases in high - risk infants using urease pretreat-ment-gas chromatography-mass spectrometry / 中华实用儿科临床杂志

Objective To detect the incidence of inherited metabolic diseases(IMD)and disorders of metabo-lism in 4 710 high - risk infants,as well as providing basis of clinical diagnosis and treatment by using urease pretreat-ment - gas chromatography - mass spectrometry(UP - GC - MS). Methods Samples were collected from high - risk infants with IMD,after removing urea,putting in internal standard,removing protein,vacuum drying and bis (trimethyl - silyl)trifluoroacetamide / trimethyl - chlorosilane derivativing,UP - GC - MS was used to analyze compo-sitions such as organic acids,amino acids,carbohydrates,pyridoxines,purines and pyrimidines,then metabolic analysis was proceeded to refer to the normal detection value of the healthy children,finally a metabolic diagnosis was made ba-sing on the clinical data such as the high - risk clinical manifestations and general biochemical tests and other special examinations. Results In the 4 710 cases,there were 98 cases of IMD(2. 1% ),326 cases of suspected IMD(6. 9% ), 2 610 cases of metabolic disorders(55. 4% ). There were 98 cases of IMD,including 57 cases of methylmalonic aciduria,12 cases of propionic acidemia,7 cases of glutaric aciduria,5 cases of hyperphenylalaninemia,maple syrup u-rine disease and multiple carboxylase defects each,4 cases of isovaleric acidemia and 3 cases of 4 - hydroxy butyric acid urine disease. Conclusions UP - GC - MS is a effective way to diagnose IMD and metabolic disorders of infants. Common IMD in Guangdong Province include methylmalonic aciduria,propionic academia,glutaric aciduria,hyperphe-nylalaninemia,maple syrup urine disease and multiple carboxylase defects. The results of the tests can provide effective guidance for diagnosis and treatment of suspected infants.

Composición molecular de ácidos húmicos evaluada mediante pirólisis - cromatografía de gases - espectrometría de masas e hidrólisis térmica asistida y metilación en suelos altoandinos de Colombia / Molecular composition of humic acids evaluated by pyrolysis - gas chromatography - mass spectrometry and thermally assisted hydrolysis and methylation in high Colombian Andean soils / Composição molecular de ácidos húmicos avaliada mediante pirólise - cromatografia de gases - massas e hidrólise térmica assistida e metilação, em solos altoandinos em Colômbia

Se determinó la composición molecular de ácidos húmicos (AH), extraídos del horizonte 'A' de suelos altoandinos de Colombia dedicados a tres usos: bosque primario, cultivos y praderas. Los AH se obtuvieron mediante extracción secuencial de la materia orgánica humificada (MOH) con soluciones de tetraborato, pirofosfato e hidróxido de sodio (0,1N), y fueron purificados mediante diferentes procesos analíticos. Su composición molecular se determinó a través de Py-GC/MS y THMA. Los diferentes productos de la pirólisis se clasificaron atendiendo a la familia química a la que pertenecen; prevalecieron los ácidos grasos (FA) como el producto más abundante en los AH de todos los usos, mientras que los fenoles, esteroles, S-compuestos y terpenos se encontraron en menor abundancia. Se presentaron diferencias en los porcentajes de abundancia relativa de los grupos identificados, demostrando así que el cambio de uso de suelo influye en sus propiedades físicas, químicas y biológicas, por lo que se perciben diferentes grados de transformación que afectan la composición de los AH y su reactividad en el suelo.

It was determined the molecular composition of humic acids (HA) extracted from 'A' horizon in Colombian high Andean soils dedicated to three uses: primary forest, croplands and pastures. The AH were obtained by sequential extraction of humified organic matter (HOM) with tetraborate, pyrophosphate and sodium hydroxide (0.1N) solutions; HA were purified through various analytical processes. Its chemical composition was determined by Py-GC/MS and THMA. Different pyrolysis products were classified in response to the chemical family to which they belong, prevailed fatty acids (FA) as the most abundant in all AH, while phenols, sterols, terpenes and S-compounds were found in lower abundance. There were differences in the percentages of relative abundance of the identified groups, showing that the land use change influences the physical, chemical, and biological propertiers of soils that are perceived at different levels of transformation, affecting the HA composition and its reactivity in the soil.

Foi determinada a composição molecular de ácidos húmicos (AH), extraídos do horizonte 'A' dos solos altoandinos, Colômbia, surgiro a três usos: floresta primária, cultivo e pastagem. Os AH se obtiveram através de extração sequencial da Matéria Orgânica Humificada (MOH) com soluções de tetraborato, pirofosfato e hidróxido de sódio (0,1N), e foram purificados por diversos processos analíticos. A sua composição química foi determinada por Py-GC/MS e THMA. Os diferentes produtos da pirolise foram classificados atendendo à família química à que pertencem, prevaleceram os ácidos gordurosos (FA) como o produto mais abundante em todos os AH, enquanto os fenóis, esteróis, S-compostos e terpenos foram encontrados em menor abundância. Surgiram diferenças nas percentagens da abundância relativa dos grupos identificados, mostrando que a mudança de uso de solo influencia nas propriedades físicas, químicas e biológicas do solo podendo ser perceptíveis diferentes graus de transformação, que afetam a composição dos AH e sua reatividade no solo.