文章摘要
韩继永,赵砚荣,周学敏.HPLC法测定恩格列净有关物质的方法学验证[J].南京医科大学学报,2017,(1):121~125
HPLC法测定恩格列净有关物质的方法学验证
Validation of HPLC method for the determination of related substances in empagliflozin
投稿时间:2016-06-01  
DOI:10.7655/NYDXBNS20170130
中文关键词: 恩格列净  有关物质  高效液相色谱法  测定
英文关键词: empagliflozin  relatedsubstance  HPLC  determination
基金项目:国家自然科学基金(81572081)
作者单位
韩继永 南京医科大学药学院江苏 南京 211166江苏奥赛康药业股份有限公司江苏 南京 211112 
赵砚荣 江苏奥赛康药业股份有限公司江苏 南京 211112 
周学敏 南京医科大学药学院江苏 南京 211166 
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中文摘要:
      目的:建立恩格列净原料药纯度及所含杂质的测定方法。方法:采用高效液相色谱(HPLC)法,用Waters symmetry C18色谱柱(250 mm×4.6 mm,5 μm),以0.01%(V/V)三氟乙酸溶液为流动相A,乙腈为流动相B,线性梯度洗脱:0~10 min,流动相B 32%;10~50 min,流动相B 32%~95%;检测波长225 nm,流速1.0 mL/min,柱温45℃。结果:恩格列净与各杂质的分离度均>1.5,检出限均<9 ng/mL, 线性范围满足定量分析要求;重复性试验相对标准差(RSD)均<5%;供试品溶液和对照溶液在8 h内稳定性良好;各杂质的回收率为88.6%~106.1%,RSD均<10%。结论:本研究建立的方法检测灵敏度高,精密度好,可作为恩格列净原料药有关物质的控制方法。
英文摘要:
      Objective: To establish a method for determination assay of empagliflozin and related substance. Methods:HPLC method was adopted. The determination was carried out on Waters symmetry C18 column(250 mm×4.6 mm,5 μm). The mobile phase A was 0.01%(V/V) trifluoroacetic acid solution,the mobile phase B was acetonitrile,linearity gradient elution was as follows:0~10 min,mobile B 32%;10~50min,mobile B 32%~95%, at a flow rate of 1.0 mL/min. The detective wavelength was set at 225 nm, and the column temperature was at 45℃. Results:The separation between empaliflozin and its related substances was not less than 1.5. The LOQ was less than 9 ng/mL,and linear range were suitbale for determination. The RSD of repeatability was less than 5.0%. The test solution and reference solution had a good stability in 8 h, the recovery of the impurities was 88.6%~106.1%, and RSD was less than 10%. Conclusion:The method is sensitive and accurate, and is effective for quality control in empagliglozin.
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