Determination Of Sulpiride Research Articles

Ultraviolet spectrophotometry for determination of sulpiride in serum

目的 建立生物样品中舒必利定性、定量测定的紫外分光光度法,为临床舒必利中毒提供诊疗依据.方法 取0.5 ml血清(或胃液)加三氯甲烷:异丙醇=95:5的有机溶剂萃取液4.0 ml,充分振荡萃取,高速离心,取有机层于另一试管中,在50℃水浴中氮气吹干,加0.2 ml甲醇溶解,取50 μl上机测定.结果 血清和胃液中舒必利最大吸收峰为(292±1) nm,血清浓度在20.0～100.0 μg/ml范围内呈线性,回归方程y=0.009 85x+0.018 3,相关系数为0.999 8,方法回收率为85.8％～103.8％,相对标准偏差(RSD)为3.3％～4.9％.日内、日间RSD分别为3.87％～4.97％和3.86％～4.84％,最低检出浓度10.0 μg/ml.结论 该方法操作简便、分析快速,结果准确.为临床诊断舒必利中毒提供了简便准确的检测方法。

Effective determination of a pharmaceutical, sulpiride, in river water by online SPE-LC–MS using a molecularly imprinted polymer as a preconcentration medium

We report an effective and a quantitative analysis method for one of pharmaceuticals, sulpiride, in river water by online solid phase extraction (SPE) connected with liquid chromatography–mass spectrometry (LC–MS) using a molecularly imprinted polymer as a preconcentration medium. The polymer prepared with a pseudo template molecule showed the selective retention ability based on the interval recognition of functional groups in sulpiride. Also, the imprinted polymer provided an effective concentration of a trace level of sulpiride in offline SPE with dual washing processes using water and acetonitrile, although another imprinted polymer prepared by an authentic method using sulpiride and methacrylic acid as a template and a functional monomer, respectively, showed the selective adsorption only in organic solvents. Furthermore, we employed the imprinted polymer as the preconcentration column of online SPE-LC–MS and the results supposed that the proposed system allowed the quantitative analysis of sulpiride with high sensitivity and recovery (10ng/L at 96%). Additionally, the determination of sulpiride in real river water without an additional spiking was effectively achieved by the system.

Determination of sulpiride in pharmaceutical preparations and biological fluids using a Cr (III) enhanced chemiluminescence method

A highly sensitive and simple method for identifying sulpiride in pharmaceutical formulations and biological fluids is presented. The method is based on increased chemiluminescence (CL) intensity of a luminol-H2O2 system in response to the addition of Cr (III) under alkaline conditions. The CL intensity of the luminol-H2O2-Cr (III) system was greatly enhanced by the addition of sulpiride and the CL intensity was proportional to the concentration of sulpiride in a sample solution. Various parameters affecting the CL intensity were systematically investigated and optimized for determination of the sulpiride in a sample. Under the optimum conditions, the CL intensity was proportional to the concentration of sulpiride in the range of 0.068-4.0 µg/mL, with a good correlation coefficient of 0.997. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 8.50 × 10(-6) µg/mL and 2.83 × 10(-5) µg/mL, respectively. The method presented here produced good reproducibility with a relative standard deviation (RSD) of 2.70% (n = 7). The effects of common excipients and metal ions were studied for their interference effect. The method was validated statistically through recovery studies and successfully applied for the determination of sulpiride in pure form, pharmaceutical preparations and spiked human plasma samples. The percentage recoveries were found to range from 99.10 to 100.05% for pure form, 98.12 to 100.18% for pharmaceutical preparations and 97.9 to 101.4% for spiked human plasma.

Development and Validation of Micellar-Enhanced Spectrofluorimetric Method for Determination of Sulpiride in Pharmaceutical Formulations and Biological Samples

Abstract Sensitive and simple spectrofluorometric method has been developed and validated for the quantification of sulpiride in pure, commercial formulations, human plasma and urine in the presence of sodium dodecyl sulphate (SDS) surfactant micelle. The experimental parameters like buffer, surfactant type and volume were studied. A linear relationship was found between sulpiride concentration and fluorescence intensity in the range of 0.02 μg mL–1–7.0 μg mL–1 containing 0.2 M sodium dodecyl sulphate with λex 292 nm and λem 343 nm with a correlation coefficient of 0.9987. The limit of detection (LOD) and limit of quantification (LOQ) was found to be 1.9 × 10–2 μg mL–1 and 5.9 × 10–2 μg mL–1 respectively. The proposed method was successfully applied for the determination of sulphiride in pure and dosage form; the percentage recoveries agreed well with the label value. The effect of common excipients used as additive in pharmaceutical formulations was studied and no interferences was found. Similarly the effect of some common cations and compounds present in urine and plasma were also investigated and the method was found free of interferences. The method was further extended to the in-vitro determination of sulphiride in spiked human plasma and urine samples with percentage recoveries from 98.33%–99.75% and 95.67%–101.67% respectively. The results of the proposed method have been compared with the literature HPLC method and no significant difference was found between them.

Solid-Phase Extraction and Determination of Sulpiride in Human Serum by High Performance Liquid Chromatography Using Electrogenerated Chemiluminescence Detection

A high performance liquid chromatography method using chemiluminescence for the determination of sulpiride in human serum was developed. The separation method employed a TSKgel ODS-80Ts column and a mobile phase containing 20% acetonitrile and 300 mM acetate buffer (pH 5.5). The reagent solution was 1 mM tris(2,2′-bipyridine)rutheniumu(II) in 10 mM sulfuric acid. Solid-phase extraction of sulpiride and tiapride added to human serum samples was performed with an Oasis® HLB cartridge column. The recovery and limit of detection of sulpiride was between 88.8 ± 7.1 and 95.2 ± 5.7%, and 1 ng/mL (0.02 ng on column) (S/N = 3), respectively. The calibration curve for sulpiride showed good linearity over the range 20–500 ng/mL. Finally, the method was applied to the determination of sulpride in human serum samples obtained after a 100 mg oral dose of sulpiride.

Studies on intestinal absorption of sulpiride (1): carrier-mediated uptake of sulpiride in the human intestinal cell line Caco-2.

We investigated whether the uptake of a specific antipsychotic agent, sulpiride, in Caco-2 cells is mediated by a carrier-mediated system. Caco-2 cell monolayers were cultured in plastic culture dishes and uptake and efflux studies were conducted. The determination of sulpiride was performed by HPLC. At 37 degrees C, sulpiride uptake in pH 6.0 was twice as much as in pH 7.4. At 4 degrees C, however, no significant difference was observed between pH 6.0 and 7.4. The uptake at 4 degrees C was markedly lower than that obtained at 37 degrees C. The subtraction of the uptake at 4 degrees C from the uptake at 37 degrees C indicated a saturable process, and the result of the Eadie-Hofstee plot analysis indicated that the uptake consists of two or more saturable components. The uptake was significantly inhibited by uncoupler, protonophore, amino acid modifying agent and proteinase. Sulpiride efflux was temperature-dependent and was significantly inhibited by uncoupler and amino acid modifying agent. These findings indicate that sulpiride uptake and efflux in Caco-2 cells are carrier-mediated. Furthermore, the uptake was significantly decreased by some substrates and inhibitors of peptide transporter, PEPT1, and organic cation transporters, OCTN1 and OCTN2, and was significantly increased by preloading with them. The uptake was also significantly increased by a typical substrate of P-glycoprotein. From these findings, we presumed that peptide transporter PEPT1 and organic cation transporters OCTN1 and OCTN2 are involved with this uptake. P-glycoprotein may also contribute to the efflux of sulpiride.