Berecka Anna, Gumieniczek Anna, Hopkała Hanna
Medical University of Lublin, Faculty of Pharmacy, Department of Medicinal Chemistry, Jaczewskiego Str. 4, 20-090 Lublin, Poland.
J AOAC Int. 2006 Mar-Apr;89(2):319-25.
A new high-performance liquid chromatography method was developed and validated for the quantitation of gliclazide and repaglinide in pharmaceutical formulations. Determination was performed using a LiChroCART RP-18 column, a mobile phase containing acetonitrile-phosphate buffer (pH 2.1; 60 + 40, v/v), and ultraviolet (UV) detection at 225 nm. Repaglinide was used as an internal standard for gliclazide determination and gliclazide for repaglinide assay. The method was validated with respect to linearity, precision, robustness, ruggedness, accuracy, and specificity. The calibration graphs ranged from 0.015 to 0.09 mg/mL for gliclazide and 0.06 to 0.36 mg/mL for repaglinide. Intra- and interday relative standard deviation values for the standard solutions were 0.70 and 1.01% for gliclazide and 0.78 and 0.93% for repaglinide, respectively. Total recoveries of gliclazide and repaglinide from the laboratory-prepared mixtures were 99.82 +/- 0.58 and 101.50 +/- 0.46% for gliclazide and repaglinide, respectively [mean +/- standard deviation (SD)]. In forced degradation studies, the effect of acid, base, oxidation, UV light, and temperature on both drugs was also investigated. Finally, the method was applied for the quality control of commercial gliclazide and repaglinide tablets. Total recovery was 100.40 +/- 0.35 and 104.46 +/- 0.23% for gliclazide and repaglinide, respectively (mean +/- SD).
开发并验证了一种用于定量药物制剂中格列齐特和瑞格列奈的高效液相色谱新方法。采用LiChroCART RP - 18柱进行测定，流动相为含乙腈 - 磷酸盐缓冲液（pH 2.1；60 + 40，v/v），在225 nm处进行紫外（UV）检测。瑞格列奈用作格列齐特测定的内标，格列齐特用作瑞格列奈测定的内标。该方法在线性、精密度、稳健性、耐用性、准确度和特异性方面进行了验证。格列齐特的校准曲线范围为0.015至0.09 mg/mL，瑞格列奈的校准曲线范围为0.06至0.36 mg/mL。标准溶液的日内和日间相对标准偏差值，格列齐特分别为0.70%和1.01%，瑞格列奈分别为0.78%和0.93%。从实验室制备的混合物中回收的格列齐特和瑞格列奈的总回收率，格列齐特为99.82±0.58%，瑞格列奈为101.50±0.46%[平均值±标准偏差（SD）]。在强制降解研究中，还研究了酸、碱、氧化、紫外光和温度对两种药物的影响。最后，该方法应用于市售格列齐特和瑞格列奈片剂的质量控制。格列齐特和瑞格列奈的总回收率分别为100.40±0.35%和104.46±0.23%（平均值±SD）。
