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1.
J Sep Sci ; 43(24): 4469-4479, 2020 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-33048447

RESUMEN

In the present work, nickel-1,4-benzenedioxyacetic acid was synthesized as a rod-like metal organic material and then modified with alumina nanoparticles to synthesize nickel metal organic modified-Al2 O3 nanoparticles. The material was found as an efficient sorbent for the enrichment of atorvastatin in human blood plasma. After the extraction of the sample of plasma by ultrasound-assisted dispersive solid phase extraction, high performance liquid chromatography-ultraviolet was used to determine the quantitatively pre-concentrated interest analyte. The conditions for optimum extraction were achieved by the optimization of the volume of eluent, dosage of the sorbent, and time of sonication. Solution pH of 7.0, 250 µL of ethanol, 45 mg of the sorbent, and 10 min of sonication time were the conditions for extracting the atorvastatin maximum recovery of higher than 97.0%. By using desirability function for the optimization of the process, the present method showed a response that was linear ranging from 0.2 to 800 ng/mL with regression coefficient of 0.999 in the plasma of human blood with a satisfactory detection limit of 0.05 ng/mL, while the precision of interday for the current method was found to be <5%. It can be concluded that dispersive solid phase extraction method is effective for the extraction of atorvastatin from human plasma samples (97.4-102%) due to its easy operation, simplicity, repeatability, and reliability.


Asunto(s)
Óxido de Aluminio/química , Atorvastatina/sangre , Estructuras Metalorgánicas/química , Nanopartículas/química , Extracción en Fase Sólida , Ondas Ultrasónicas , Ácido Acético/química , Cromatografía Líquida de Alta Presión , Humanos , Estructuras Metalorgánicas/síntesis química , Níquel/química , Tamaño de la Partícula
2.
J Pharm Biomed Anal ; 149: 166-171, 2018 Feb 05.
Artículo en Inglés | MEDLINE | ID: mdl-29121570

RESUMEN

In this research, a facile and selective method was described to extract l-cysteine (l-Cys), an essential α-amino acid for anti-ageing playing an important role in human health, from human blood plasma sample. The importance of this research was the mild and time-consuming synthesis of zinc organic polymer (Zn-MOP) as an adsorbent and evaluation of its ability for efficient enrichment of l-Cys by ultrasound-assisted dispersive micro solid-phase extraction (UA-DMSPE) method. The structure of Zn-MOP was investigated by FT-IR, XRD and SEM. Analysis of variance (ANOVA) was applied for the experimental data to reach the best optimum conditions. The quantification of l-Cys was carried out by high performance liquid chromatography with UV detection set at λ=230nm. The calibration graph showed reasonable linear responses towards l-Cys concentrations in the range of 4.0-1000µg/L (r2=0.999) with low limit of detection (0.76µg/L, S/N=3) and RSD≤2.18 (n=3). The results revealed the applicability and high performance of this novel strategy in detecting trace l-Cys by Zn-MOP in complicated matrices.


Asunto(s)
Cisteína/sangre , Estructuras Metalorgánicas/química , Microextracción en Fase Sólida/métodos , Zinc/química , Adsorción , Envejecimiento/sangre , Análisis de Varianza , Cromatografía Líquida de Alta Presión/instrumentación , Cromatografía Líquida de Alta Presión/métodos , Cisteína/química , Estudios de Factibilidad , Humanos , Límite de Detección , Estructuras Metalorgánicas/ultraestructura , Microscopía Electrónica de Rastreo , Difracción de Polvo/instrumentación , Difracción de Polvo/métodos , Espectroscopía Infrarroja por Transformada de Fourier/instrumentación , Espectroscopía Infrarroja por Transformada de Fourier/métodos , Propiedades de Superficie , Ondas Ultrasónicas , Difracción de Rayos X/instrumentación , Difracción de Rayos X/métodos
3.
Artículo en Inglés | MEDLINE | ID: mdl-28987498

RESUMEN

In present work, facile method is developed for determination of colchicine in human plasma sample, autumn and spring root of colchicium extracts by ultrasound assisted dispersive magnetic solid phase microextraction followed by HPLC-UV method (UAD-MSPME-HPLC-UV). Magnetic (Fe2O4-nanoparticles) metal organic framework-5, (MOF-5(Zn)-Fe2O4NPs) was synthesized by dispersing MOF-5 and Fe(NO3)3.9H2O in ethylene glycol (as capping agent) and NaOH (pH adjustment agent) by hydrothermal method. The prepared sorbent was characterized via XRD and SEM analysis and applied as magnetic solid phase in UAD-MSPME-HPLC-UV method. In this method, colchicine molecules were sorbed on MOF-5(Zn)-Fe2O4NPs sorbent by various mechanisms like ion exchange, hydrogen bonding and electrostatic, á´¨-á´¨, hard-hard and dipole-ion interaction followed by exposing sonication waves as incremental mass transfer agent and then the sorbent was separated from the sample matrix by an external magnetic fields. Subsequently, accumulated colchicine were eluted by small volume of desorption organic solvent. Influence of operational variables such as MOF-5(Zn)-Fe2O4NPs mass, volume of extracting solvent and sonication time on response property (recovery) were studied and optimized by central composite design (CCD) combined with desirability function (DF) approach. Under optimum condition, the method has wide linear calibration rang (0.5-1700ngmL-1) with reasonable detection limit (0.13ngmL-1) and R2=0.9971. Finally, the UAD-MSPME-HPLC-UV method was successfully applied for determination of colchicine autumn and spring root of colchicium extracts and plasma samples.


Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Colchicina , Colchicum/química , Nanocompuestos/química , Extractos Vegetales/química , Microextracción en Fase Sólida/métodos , Colchicina/análisis , Colchicina/química , Colchicina/aislamiento & purificación , Óxido Ferrosoférrico/química , Concentración de Iones de Hidrógeno , Límite de Detección , Modelos Lineales , Raíces de Plantas/química , Reproducibilidad de los Resultados , Compuestos de Zinc/química
4.
Ultrason Sonochem ; 34: 317-324, 2017 01.
Artículo en Inglés | MEDLINE | ID: mdl-27773252

RESUMEN

The present research focus on designing an appropriate dispersive solid-phase microextraction (UA-DSPME) for preconcentration and determination of Eriochrome Cyanine R (ECR) in aqueous solutions with aid of sonication using lead (II) dioxide nanoparticles loaded on activated carbon (PbO-NPs-AC). This material was fully identified with XRD and SEM. Influence of pH, amounts of sorbent, type and volume of eluent, and sonication time on response properties were investigated and optimized by central composite design (CCD) combined with surface response methodology using STATISTICA. Among different solvents, dimethyl sulfoxide (DMSO) was selected as an efficient eluent, which its combination by present nanoparticles and application of ultrasound waves led to enhancement in mass transfer. The predicted maximum extraction (100%) under the optimum conditions of the process variables viz. pH 4.5, eluent 200µL, adsorbent dosage 2.5mg and 5min sonication was close to the experimental value (99.50%). at optimum conditions some experimental features like wide 5-2000ngmL-1 ECR, low detection limit (0.43ngmL-1, S/N=3:1) and good repeatability and reproducibility (relative standard deviation, <5.5%, n=12) indicate versatility in successful applicability of present method for real sample analysis. Investigation of accuracy by spiking known concentration of ECR over 200-600ngmL-1 gave mean recoveries from 94.850% to 101.42% under optimal conditions. The procedure was also applied for the pre-concentration and subsequent determination of ECR in tap and waste waters.


Asunto(s)
Bencenosulfonatos/aislamiento & purificación , Carbón Orgánico/química , Plomo/química , Óxidos/química , Microextracción en Fase Sólida/métodos , Sonicación , Purificación del Agua/métodos , Agua/química , Adsorción , Bencenosulfonatos/química , Nanopartículas/química , Contaminantes Químicos del Agua/química , Contaminantes Químicos del Agua/aislamiento & purificación
5.
Int J Gynecol Cancer ; 23(5): 809-14, 2013 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-23574882

RESUMEN

OBJECTIVE: In immunotherapy of HPV-16-associated cervical cancers, the E7 protein is considered as a prime candidate. However, it is a poor inducer of a cytotoxic T-cell response when used as a singular antigen in protein vaccination. Therefore, to design effective cancer vaccines, the best tumor antigens should be combined with the most effective immunogens or drug delivery tools to achieve positive clinical results. In this study, we fused HPV-16 E7 with the lectin subunit of ricin toxin (RTB) from castor plant as a vaccine adjuvant/carrier. MATERIALS AND METHODS: After reaching the soluble form of the recombinant protein, we designed 2 preventive and inhibition tumor models for investigation of the prevention and rejection of TC-1 cell growth in female C57BL/6 mice, respectively. In each model, mice were immunized with the recombinant protein of E7-RTB or E7 without any adjuvant. RESULTS: We demonstrated that prophylactic immunization of E7-RTB protected mice against challenge from TC-1 cells. Also in the therapeutic model, E7-RTB could inhibit TC-1 tumor growth in the lung. The results were significant compared with the immunization of E7 singularly. CONCLUSIONS: We concluded that immunization with E7-RTB protein without any adjuvant could generate antitumor effects in mice challenged with TC-1 cells. This research verifies the clinical applications and the future prospects for development of HPV-16 E7 therapeutic vaccines fused to immunoadjuvants.


Asunto(s)
Vacunas contra el Cáncer/uso terapéutico , Inmunoterapia , Proteínas E7 de Papillomavirus/inmunología , Proteínas Recombinantes de Fusión/inmunología , Ricina/inmunología , Linfocitos T Citotóxicos/inmunología , Neoplasias del Cuello Uterino/prevención & control , Animales , Ensayo de Inmunoadsorción Enzimática , Femenino , Humanos , Inmunización , Ratones , Ratones Endogámicos C57BL , Proteínas E7 de Papillomavirus/genética , Proteínas E7 de Papillomavirus/metabolismo , Proteínas Recombinantes de Fusión/genética , Proteínas Recombinantes de Fusión/metabolismo , Ricina/genética , Ricina/metabolismo , Linfocitos T Citotóxicos/metabolismo , Neoplasias del Cuello Uterino/inmunología , Neoplasias del Cuello Uterino/metabolismo
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