摘要
目的:建立高效液相色谱-质谱法测定伏格列波糖片中伏格列波糖的含量。方法:采用Agilent ZORBAX Eclipse Plus C18(2.1 mm ×150 mm,3.2μm)色谱柱,柱温40℃,流速为0.25 ml/min,甲醇-水(2∶3)为流动相,流速为0.25 ml/min,质谱检测中采用电喷雾离子源多反应检测扫描( MRM)模式。结果:伏格列波糖浓度在1.5804~2.6340μg/ml范围内线性关系良好,其中离子对268.2/74.2(r=0.9990)平均回收率为100.2%,相对标准偏差为1.37%( n=6);离子对268.2/92.2(r=0.9976)平均回收率为99.3%,相对标准偏差为1.78%(n=6)。结论:高效液相色谱-质谱法准确性、重复性均好,可用于伏格列波糖片的质量控制。
Objective:To develop a method for determination of voglibose contents in its tablets by high-performance liquid chromatography-mass spectrometry ( HPLC-MS) .Methods:The measurements were carried out on an Agilent ZORBAX Eclipse Plus C18 column (2.1 ×150mm 3.2μm) with a temperature of 40℃.A mixture of methanol and water (2∶3, v/v) was used as a mobile phase at a flow rate of 0.25 ml/min.Voglibose was detected in an electrospray ionization (ESI) mode with MRM. Results:The calibration curves of voglibose showed good linearity in a range of 1 .5804-2.6340 μg/ml (r=0.9990).The average recovery was 100.2%with RSD of 1.37%( n=6 ) for m/z 268 .2/74 .2 .Linearity was obtained with r=0 .9976 and the average recovery was 99.3%with RSD of 1.78%(n=6) for m/z 268.2/92.2.Conclusion:HPLC-MS method is accurate , reproducible and can be used for quality control of voglibose tablets .
出处
《浙江大学学报(医学版)》
CAS
CSCD
北大核心
2014年第2期141-144,共4页
Journal of Zhejiang University(Medical Sciences)
关键词
肌醇
分析
肌醇
类似物和衍生物
回收率
温度
色谱法
高压液相
质谱分析法
伏格列波糖
Inositol/analysis
Inositol/analogs & derivatives
Retrieving rate
Temperature
Chromatography,high pressure liquid
Mass spectrometry
Voglibose