Lakshmi Karunanidhi Santhana, Rajesh Tirumala
Department of Pharmaceutical Analysis, SRM College of Pharmacy, SRM University, Kattankulathur-603203, Tamil Nadu, India.
PDA J Pharm Sci Technol. 2011 Mar-Apr;65(2):100-8.
A rapid and sensitive high performance liquid chromatography-mass spectrometry method has been developed for quantitative determination of Rosiglitazone, a thiazolidinedione drug used for the treatment of type II diabetes mellitus in rat plasma. The method was also validated as per International Conference on Harmonization (ICH) and Food and Drug Administration (FDA) guidelines. The analyte was extracted from rat plasma by the simple precipitation of plasma proteins technique using acetonitrile as a precipitating agent. Alprazolam was used as the internal standard. A Chromolith RP-18(e) column provided chromatographic separation of the analyte using a mobile phase containing 5mM ammonium acetate in water (pH 3) and methanol (20:80) at a flow rate of 1 mL/min with an elution time as low as 2.5 min, which was followed by detection with mass spectrometry. The mass transition ion-pair was followed as m/z 358.0 for rosiglitazone and m/z 308.8 for alprazolam. Simple isocratic chromatographic conditions and mass spectrometric detection of the method enable the detection of rosiglitazone at less than nanogram levels. The proposed method was found to be linear from 0.5 to 100 ng/mL (r(2) = 0.9987). The percent coefficient of variance for precision and accuracy values found at LLOQ (9.17), LQC (8.45), MQC (1.66) and HQC (1.53). The overall recovery of rosiglitazone was 95.9%. The developed and validated method was successfully applied for the pharmacokinetic studies of rosiglitazone tablets after a single oral dose to healthy Wistar rats.
A rapid and sensitive high performance liquid chromatography-mass spectrometry method has been developed and validated for quantification of rosiglitazone in rat plasma. The analyte was extracted from rat plasma by simple precipitation technique. Alprazolam was used as the internal standard. A Chromolith RP-18(e) column provided chromatographic separation of the analyte using a mobile phase containing 5mM ammonium acetate in water and methanol (20:80) at a flow rate of 1 mL/min which was followed by detection with mass spectrometry. The mass transition ion-pair was followed as m/z 358.0 for rosiglitazone and m/z 308.8 for alprazolam. The method involves precipitation of rosiglitazone from plasma, simple isocratic chromatography conditions and mass spectrometric detection that enables detection at less than nanogram levels. The proposed method has been validated with a linear range of 0.5 to100 ng/mL for rosiglitazone. The percent coefficient of variation for precision and accuracy are within 10%. The overall recovery of rosiglitazone was 95.9%. Total elution time was as low as 2.5 min. The developed and validated method was successfully applied for the pharmacokinetic studies of rosiglitazone tablets after a single oral dose to rats.
已开发出一种快速灵敏的高效液相色谱 - 质谱法，用于定量测定罗格列酮，罗格列酮是一种噻唑烷二酮类药物，用于治疗大鼠血浆中的II型糖尿病。该方法也按照国际协调会议（ICH）和美国食品药品监督管理局（FDA）的指南进行了验证。通过使用乙腈作为沉淀剂的血浆蛋白简单沉淀技术从大鼠血浆中提取分析物。阿普唑仑用作内标。使用Chromolith RP - 18(e)柱，以1 mL/min的流速，采用含5 mM醋酸铵的水溶液（pH 3）和甲醇（20:80）的流动相进行分析物的色谱分离，洗脱时间低至2.5分钟，随后进行质谱检测。罗格列酮的质量转移离子对为m/z 358.0，阿普唑仑的质量转移离子对为m/z 308.8。该方法简单的等度色谱条件和质谱检测能够检测到纳克以下水平的罗格列酮。所提出的方法在0.5至100 ng/mL范围内呈线性（r(2) = 0.9987）。在LLOQ（9.17）、LQC（8.45）、MQC（1.66）和HQC（1.53）下测得的精密度和准确度值的变异系数百分比。罗格列酮的总回收率为95.9%。所开发和验证的方法成功应用于健康Wistar大鼠单次口服罗格列酮片后的药代动力学研究。
已开发并验证了一种快速灵敏的高效液相色谱 - 质谱法，用于定量测定大鼠血浆中的罗格列酮。通过简单沉淀技术从大鼠血浆中提取分析物。阿普唑仑用作内标。使用Chromolith RP - 18(e)柱，以1 mL/min的流速，采用含5 mM醋酸铵的水溶液和甲醇（20:80）的流动相进行分析物的色谱分离，随后进行质谱检测。罗格列酮的质量转移离子对为m/z 358.0，阿普唑仑的质量转移离子对为m/z 308.8。该方法包括从血浆中沉淀罗格列酮、简单的等度色谱条件和质谱检测，能够检测到纳克以下水平。所提出的方法已针对罗格列酮在0.5至100 ng/mL的线性范围进行了验证。精密度和准确度的变异系数百分比在10%以内。罗格列酮的总回收率为95.9%。总洗脱时间低至2.5分钟。所开发和验证的方法成功应用于大鼠单次口服罗格列酮片后的药代动力学研究。
