Residues determination of oxytetracycline, tetrarcycline and chlortetracycline in zaosheng cattle meat by SPE-HPLC / 国际药学研究杂志

Objective To establish a method for simultaneous determination of 3 tetracyline antibiotics (TCs) oxytetra-cycline (OTC), tetracycline (TC), chlorotetecycline (CTC)) residues in Zaosheng cattle meat using solid phase extraction-high performance liquid chromatography (SPE-HPLC). Methods The samples were extracted by Na2EDTA-Mcllvaine buffer solution (pH=4.0), and 15% trichloroacetic acid (TCA) as the protein precipitation solution, then the targets were cleaned up and enriched by C18 solid phase extraction column. HPLC Mobile phase consisted of oxalic acid (0.01mol/L), acetonitrile as well as methanol. The detection wavelength was 350 nm and external standard method was adopted for quantification. Results The calibration curves of 3 TCs had good linearity with correlation coefficients of 0.998. The limits of detection of OTC, TC and CTC were 18, 15, 30 μg/kg, respectively, while their average recoveries were 76.10%-95.22%, with relative standard deviations (RSD) lower than 10% after optimized pretreatment and analytical conditions. Conclusion The method has high sensitivity, precision, and good repeatability, and can meet the needs of residue determination of TCs in meat.

Determination of Two Components in Shangyangyu Ointment by Solid Phase Extraction Coupled with HPLC Method / 中国药师

To develop a determination method forβ,β'-dimethylacrylalkannin and salvianolic acid B in Shangyangyu ointment by solid phase extraction coupled with HPLC. Methods:Solid phase extraction coupled with HPLC was used with a C18 (250 mm × 4. 6 mm, 5 μm) column, the mobile phase was acetonitrile-water-methanol-formic acid (700∶300∶30∶15) with the flow rate of 1. 0 ml·min-1. For β, β'-dimethylacrylalkannin, the detection wavelength was 275nm, and for salvianolic acid B, the detection wavelength was 286nm. Under the above conditions, the contents of main componentsβ,β'-dimethylacrylalkannin and salvianolic acid B in Shangyangyu ointment were determined. Results:The linear relationship was promising when the concentration ofβ,β'-dimethyl-acrylshikonin was within the range of 23. 780-118. 900μg·ml-1(r=0. 999 5) with the recovery of 99. 5% (RSD=1. 07%) and that of salvianolic acid B was within the range of 19.840-99.200 μg·ml-1(r=0.999 3) with the recovery of 98.2% (RSD=2.1%). Conclusion:The method is simple, accurate and fast with good separation, which can be used in the quality control of Shangyangyu ointment.

Avaliação da remoção de interferentes endócrinos, ativos farmacêuticos e cafeína em água para abastecimento público do estado de São Paulo / Assessment of endocrine disruptors, pharmaceuticals and caffeine removal in drinking water of the São Paulo State

Alguns compostos orgânicos como interferentes endócrinos e ativos farmacêuticos estão sendo encontrados em águas superficiais e vêm chamando a atenção de orgãos públicos e da comunidade científica. Dentre esses compostos, foram enfatizados nesse trabalho, o hormônio sintético 17α-etinilestradiol, o surfactante (4-nonilfenol), bisfenol A, o antibiótico ß-lactâmico amoxicilina e a cafeína como traçador de atividade antrópica. Estes compostos são continuamente introduzidos em corpos d'água pelo lançamento de esgoto in natura o que afeta a qualidade da água, a saúde dos ecossistemas e impacta o suprimento de água potável. Considerando a baixa taxa de remoção desses contaminantes pelo tratamento de água atualmente utilizado no Brasil e o estado de degradação dos mananciais de água para abastecimento público, esse trabalho apresenta o desenvolvimento de metodologia analítica para determinação dos compostos citados e a avaliação da eficiência de remoção quando o tratamento convencional de água é aplicado. A determinação foi baseada em métodos já estabelecidos e envolveram as etapas de limpeza e concentração de amostra usando extração em fase sólida (SPE) e análise por cromatografia a líquido de alta eficiência (HPLC) com detector de arranjo de diodos (DAD) e espectrometria de massas. As amostras do Reservatório do Guarapiranga foram utilizadas para ensaios em escala laboratorial que simulavam o tratamento convencional de água em planta real. Os resultados mostraram a adequação dos métodos utilizados para a separação e determinação desses compostos em amostras ambientais. Além disso, apontaram para a necessidade de se avaliar a utilização de metodologias não convencionais que otimizem a remoção pelo tratamento de água atualmente utilizado

Some organic compounds, such as endocrine disruptors and pharmaceuticals, are being found in the surface water, and are concerning both the public organs and the scientific community. Among these compounds, the synthetic hormone 17α-ethinylestradiol, the surfactant (4-nonylphenol), bisphenol-A, the ß-lactam antibiotic amoxicillin and the marker of human activity caffeine were highlighted in the present work. These compounds are continuously drained to the water bodies by sewers, affecting not only the water quality itself, but also the ecosystems, and impacting the drinking water availability. Currently in Brazil, the removal rate of these contaminants is low, whereas the water sources for public supply are highly degraded. In this context, the present work develops an analytical method to detect the aforementioned compounds, and to evaluate the efficiency of its removal by conventional water treatments. Detection was based on pre-established methods and steps involved clean up and samples concentration by solid phase extraction (SPE), high performance liquid chromatography with diode array detection (DAD), and mass spectrometry. Recovery tests were done using environmental samples from Guarapiranga Reservoir (São Paulo, SP). This samples were further used in laboratorial tests, simulating real scale water conventional treatments. Current results revealed the adequacy of the chosen methods in the separation and determination of the abovementioned compounds from natural samples. Also, they highlight the need for the evaluation of non-conventional methodologies that optimize removal by current water treatment

Residuos de plaguicidas en aguas para consumo humano en una comunidad agrícola del estado Mérida, Venezuela / Pesticide residues in drinking water of an agricultural community in the state of Mérida, Venezuela

El objetivo del presente trabajo fue determinar la presencia de plaguicidas en agua potable, provenientes de seis acueductos en una región de intensa actividad agrícola del Estado Mérida, Venezuela. El estudio fue realizado durante cuatro semanas continuas, entre mayo y junio de 2008. Los residuos de plaguicidas fueron analizados mediante extracción en fase sólida y HPLC con detector de arreglo de diodos. El método SPE-HPLC-DAD cumplió con los criterios de validación analítica: linealidad (R²: 0,9840-0,9999), precisión (coeficiente de variabilidad inter-día 1,47-6,25%), exactitud (desviación estándar relativa 0,9-9,20%) y sensibilidad (límite de detección ≤ 0,012 µg/L; límite de cuantificación ≤ 0,030 µg/L, excepto mancozeb con 0,400 µg/L). Siete de los trece plaguicidas seleccionados tienen un porcentaje de recuperación entre 100% y 70%, el resto, entre 61% y 37%. En 72 muestras analizadas, se detectaron diez plaguicidas de los grupos químicos: organofosforados, carbamatos, triazinas y derivados de urea. Los plaguicidas con mayor frecuencia de detección fueron: carbofuran y atrazina (39%), malation (25%), dimetoato y metribuzin (19%). Los plaguicidas que se encontraron en niveles más altos fueron: diazinon (26,31 µg/L), metamidofos (10,99 µg/L), malation (2,03 µg/L) y mancozeb (1,27 µg/L). Los niveles de plaguicidas no superaron los valores máximos permitidos por la Legislación Venezolana, sin embargo, fueron superiores al nivel máximo permitido por la Unión Europea y EPA-USA. Este estudio demuestra la urgente necesidad de hacer un monitoreo sistemático de la calidad del agua para consumo humano en las regiones de alta productividad agrícola.

The aim of this study was to determine the presence of pesticides in drinking water from six aqueducts in a region of intense agricultural activity in the state of Merida, Venezuela. The study was conducted for four continuous weeks, between May and June 2008. Pesticide residues were analyzed by solid phase extraction (SPE) and liquid chromatography (HPLC) with diode array detector (DAD). The method SPE-HPLC-DAD met the criteria of analytical validation, with good linearity (R²: 0.9840 to 0.9999), precision (coefficient of inter-day variability from 1.47 to 6.25%), accuracy (relative standard deviation 0.9 to 9.20%) and sensitivity (LOD ≤ 0.012 µg/L; LOQ ≤ 0.030 µg/L, except mancozeb with 0.400 µg/L). Seven of the thirteen selected pesticides have a recovery rate between 100% and 70%, the rest between 61% and 37%. Ten pesticides of the following chemical groups, were detected in 72 samples analyzed: organophosphates, carbamates, triazines and urea derivatives. The pesticides with the highest frequency of detection were: carbofuran and atrazine (39%), malathion (25%), dimethoate and metribuzin (19%). The pesticides found at high levels were diazinon (26.31 µg/L), methamidophos (10.99 µg/L), malathion (2.03 µg/L) and mancozeb (1.27 µg/L). Pesticide levels did not exceed the maximum allowed by Venezuelan law, however, according to international standards (EU and EPA-USA) values were above the maximum permissible levels. This study demonstrates the urgent need for systematic monitoring of the quality of water for human consumption in regions of high agricultural productivity.

Determination of the Content of Morphine in Pipazhike Soft Capsules by SEP-HPLC / 中国药房

OBJECTIVE:To establish a method for determination of Morphine in Pipazhike soft capsules by using SPE-HPLC.METHODS:SPE condition:C18 cartridge.15mL MeOH-water(3∶ 1)and 5mL water were used as elution solvent.RESULTS:Morphine had a good linearity in the rang of 0.233 5～ 1.868 0? g(r=0.999 9).The average recovery rate was 97.6%(RSD=1.2%,n=5).CONCLUSION:This method is simple,accurate,and reproducible,and can be used to effectively control the content of Morphine in Pipazhike soft capsules.

Determination of Plasma Diclofenac Sodium by SPE-HPLC / 中国药房

OBJECTIVE: To establish an SPE(solid phase extraction)-HPLC method for the determination of diclofenac sodium in human plasma.METHODS: The separation of diclofenac sodium was performed on ODS-2 column with a detection wavelength of 280nm.The mobile phase was composed of phosphate buffer(pH6.5)-methanol(40∶ 60) at a flow rate of 1.0mL? min-1.RESULTS: The linear range of diclofenac sodium was 16.2～ 2 024.0ng? mL-1(r=0.998 9).The methodological recovery ranged between 90% to 110% and the extraction recovery was above 90%.Both intraday RSD and inter-day RSD were less than 5%.CONCLUSION: The method is simple,accurate and reliable,and suitable for the pharmacokinetic study of diclofenac sodium.

Determination of taurocholic acid in Shedanchuanbei Oral Liquid and snake bile by SPE-HPLC / 中成药

Objective: To establish the method for determination of taurocholic acid in the Traditional Chinese Medicine Shedanchuanbei Oral Liquid and snake bile. Methods: The sample was prepared as mixed solution containing methanol and KH 2PO 4. The mixed solution was injected into Sep Pak C 18 cartridge for the purpose of sample purity. In this processing, the substances which having strong retain action and could harm analytic column were hold in the Sep Pak C 18 cartridge. The eluting solution that the Sep Pak C 18 cartridge had be over loading for taurocholic acid was used as the test solution. The test solution was measured by RP HPLC. The chromatographic conditions were as followed: Supelcosil LC 8 column(150mm?4.6nm,5?m) as analytic column, detect wavelength at 203nm, and MeOH 0.4%KH 2PO 4 mixed solution(56∶44, V/V ) as mobile phase. The inject volume was 50?L. Results: The linear response range of sodium taurocholate was from 0.0253mg?mL -1 to 0.253mg?mL -1 , and the correlation coefficient was 0.9999. The average recovery rate was 101.3%, RSD was 0.40%( n =6). Conclusion: This method was simple, efficient and suitable to the quality control for Shedanchuanbei Oral Liquid and snake bile.