El-Wasseef Dalia Rashad
Department of Medicinal Chemistry. Faculty of Pharmacy, Mansoura University, 35516, Mansoura, Egypt.
Int J Biomed Sci. 2012 Jun;8(2):144-51.
A micellar chromatographic method has been developed and validated for simultaneous separation and determination of metformin(MF), nateglinide (NT) and gliclazide (GL). The separation was carried out using a Nucleosil C18 column, 150 mm × 4.6 mm i.d., 5 μm particle size, using micellar mobile phase consisting of sodium dodecyl sulphate (SDS), n-propanol with UV detection. The optimum conditions for the simultaneous separation of the three drugs were 0.12 M SDS, 10% (v/v) n-popanol, 0.3% triethylamine adjusted to pH5.6 with a flow rate of 1 ml.min(-1) and detection at 254 nm. The limit of detection (LOD) of MF, NT, GL were 0.047, 0.00115, 0.036 μg.mL(-1) respectively. The method showed good linearity in the ranges of 0.4-16 μg.mL(-1), (r(2)=0.999), 0.8-16 μg.ml(-1) (r(2)=0.999) and 1-40 μg.ml(-1) (r(2)=0.999) for MF, NT, GL respectively. The suggested method was successfully applied for the analysis of the three antidiabetic drugs in pharmaceutical preparations with average recoveries of 99.66%, 100.08% and 100.31% for MT, NT and GL respectively. The results obtained were in good agreement with those obtained from comparison methods. The method was validated regarding accuracy and precision.
已开发并验证了一种胶束色谱法，用于同时分离和测定二甲双胍（MF）、那格列奈（NT）和格列齐特（GL）。分离采用粒径为5μm、内径4.6mm×150mm的Nucleosil C18柱，以十二烷基硫酸钠（SDS）、正丙醇组成的胶束流动相进行，并采用紫外检测。同时分离这三种药物的最佳条件为：0.12M SDS、10%（v/v）正丙醇、0.3%三乙胺，用pH5.6调节，流速为1ml·min⁻¹，检测波长为254nm。MF、NT、GL的检测限（LOD）分别为0.047、0.00115、0.036μg·mL⁻¹。该方法在MF、NT、GL的浓度范围分别为0.4 - 16μg·mL⁻¹（r² = 0.999）、0.8 - 16μg·mL⁻¹（r² = 0.999）和1 - 40μg·mL⁻¹（r² = 0.999）时显示出良好的线性。所建议的方法成功应用于药物制剂中三种抗糖尿病药物的分析，MT、NT和GL的平均回收率分别为99.66%、100.08%和100.31%。所得结果与比较方法获得的结果高度一致。该方法在准确性和精密度方面得到了验证。
