Determination of methyl propyl ketone in air of workplace by capillary gas chromatography / 中华劳动卫生职业病杂志

<p><b>OBJECTIVE</b>To establish a gas chromatography method for determination of methyl propyl ketone in the air of workplace.</p><p><b>METHODS</b>Methyl propyl ketone in the air of workplace was collected with activated carbon tubes and desorbed with carbon disulfide before sample loading. The target toxicant was separated with the capillary column and detected with a hydrogen flame ionization detector, identified by retention time, and quantified by peak area.</p><p><b>RESULTS</b>The linear range of methyl propyl ketone in the air of workplace was 202.5∼4 860.0 µg/ml, with a correlation coefficient of 0.999 98. The limit of detection was 1.5 µg/ml. The lower limit of quantification was 5.0 µg/ml. The minimum detectable concentration was 1.0 mg/m(3) under 1.5 L sampling volume and 1.0 ml desorption solution volume. The relative standard deviation of different methyl propyl ketone concentrations was 1.42%∼1.65%, and the recovery rate was 94.9%∼ 97.9%.</p><p><b>CONCLUSION</b>This method has high sensitivity, precision, and accuracy, and it is applicable for determination of methyl propyl ketone in the air of workplace.</p>

Validated spectrofluorimetric method for determination of sulpiride in commercial formulations using Hantzsch condensation reaction

A simple, sensitive, selective and cost effective spectrofluorimetric method has been established for the quantification of sulpiride after their complete alkaline hydrolysis. The method is based on the condensation of the primary amino group of alkaline hydrolytic product of sulpiride with acetyl acetone and formaldehyde in acidic medium [0.25 M HCl] to form a fluorescent product. The reaction product formed shows maximum fluorescence intensity at 483 nm after excitation at 431 nm. The different reaction conditions influencing the condensation reaction were carefully optimized and a linear range of 0.1-3.5 micro g mL[-1] with good correlation coefficient between florescent intensity and concentration of sulpiride was found at optimum parameters. The LOD and LOQ were found to be 11 and 39 ng mL[-1] respectively. The proposed method was successfully used for the quantification of sulpiride in bulk powder and commercial formulations. The effect of common pharmaceutical excipients and co-administered drug was also studied and no interferences were observed. The validity of the method was tested by analyzing sulpiride in bulk powder, and pharmaceutical formulations through recovery studies. Recoveries [%] were obtained from 98.62 to 100.24% for bulk powder, and 97.09 to 100.57% for commercial formulations. The results were validated statistically with those obtained by reference literature high performance liquid chromatographic method

In vitro anti-proliferation/cytotoxic activity of epingaione and its derivatives on the human SH-SY5Y neuroblastoma and TE-671 sarcoma cells / Actividad citotóxica antiproliferativa in vitro de la epingaiona y sus derivados, sobre el neuroblastoma humano sh-sy5y y las células del sarcoma te-671

Epingaione (4-Methyl-1-(5-methyl-2, 3,4,5-tetrahydro-[2,3']bifuranyl-5-yl)-pentan-2-one) was isolated as one of the major lipophilic secondary metabolites from the leaves and stems of Bontia daphnoides L. The compound gave 79.24and 50.83anti-proliferation/cytotoxic activity on the human SH-SY5Y neuroblastoma and TE-671 sarcoma cells in vitro at 50 pg/mL, respectively. Epingaione was transformed into eleven derivatives under laboratory conditions using ethanol, some gave greater anti-proliferation/cytotoxic activity on the cancer cell lines tested. One of the derivatives (compound 2) with enhanced cytotoxic activity was elucidated as 5'-Ethoxy-5-methyl-5-(4-methyl-2-oxo-pentyl)-2,3,4,5-tetrahydro-5'H-[2,3']bifuranyl-2'-one. Both epingaione and compound 2 caused an accumulation of arrested or dead SH-SY5Y neuroblastoma in the m-phase of the cell cycle as revealed by the m-phase specific marker KE 67.

La epingaiona (4-Metil-1-(5-metil-2,3,4,5-tetrahidro-[2,3']bifuranil-5-il)-pentan-2-uno) fue aislada como uno de los principales metabolitos lipofilicos secundarios de las hojas y tallos de Bontia daphnoides L. El compuesto produjo 79.24 % y 50.83 % de actividad citotóxica/anti-proliferación sobre el neuroblastoma humano SH-SY5Y y las células del sarcoma TE-671 in vitro a 50 µg/mL, respectivamente. La epingaiona fue transformada en once derivados en condiciones de laboratorio, utilizando etanol. Algunos produjeron mayor actividad citotóxica y antiproliferativa sobre las líneas celulares cancerosas sometidas a ensayo. Uno de los derivados (compuesto 2) de elevada actividad citotóxica fue identificado como 5'-Etoxi-5-metil-5-(4-metil-2-oxo-pentil)-2,3,4,5-tetrahidro-5'H- [2,3']bifuranil-2'-uno. Tanto la epingaiona como el compuesto 22 causaron una acumulación de neuroblastomas SH-SY5Y muertos o detenidos en la fase m del ciclo celular, según lo revela el marcador KE 67 específico de la fase m.

Spectrophotometric and liquid chromatographic determination of dopamine from pharmaceutical preparations using acetyl acetone as derivatizing reagent

Dopamine [DA] has been determined by spectrophotometry and by liquid chromatography as derivatives of acetylacetone [AA]. The liquid chromatography of DA was carried out in the presence of hydroxyproline [HP], octopamine [OP] and tyramine [TY]. The separation was obtained from Phenomenex C-18 column 5pm [150 x 4.6 mm id] by isocratic elution with methanol: acetonitrile: water [45: 6: 49v/v/v], UV detection was at 320nm. Linear calibration curves were obtained for each with 2.5-40.0 micro gml-1 with detection limits in the range 1.8-80ng injection-1 [10 micro l]. The dopamine was determined in pharmaceutical preparations with coefficient of variation [CV] within 0.7-1.5%

Etude de l'activite cytotoxique in vitro des derives du cyclopentanone

The cytotoxicity of 30 cyclopentanone derivatives was studied in vitro, in a clonogenic assay using murine leukemia LI 210. Results are compared to those obtained with reference medicaments. 17 derivatives exhibit activities against L1 210 cells.