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目的:建立HPLC方法准确测定格列喹酮片的含量,解决现行质量标准中含量测定方法不专属、供试品溶液配制方法不合理的问题。方法:采用UPLC-MS联用技术对降解杂质进行分析,正负离子同时扫描和子离子扫描模式,色谱柱为ACQUITY UPLC BEH C18柱(50 mm×2.1 mm,1.7μm),流动相为水(用甲酸调节pH至3.5)(A)-乙腈(B)梯度洗脱。采用建立的HPLC法对格列喹酮片的含量进行测定,Agilent Zorbax SB-C18色谱柱(150 mm×4.6 mm,5μm),流动相为水(用甲酸调节pH至3.5)-乙腈(37.5∶62.5),检测波长为230 nm,柱温30℃,流速为1.0 ml·min-1,进样体积为20μl。结果:格列喹酮在60.200~140.400μg·ml-1范围内与峰面积线性关系良好(r=0.999 5),平均回收率为98.60%,RSD为0.6%(n=9)。结论:本方法结果准确可靠,专属性强,重复性好,可用于格列喹酮片含量及含量均匀度的测定。
OBJECTIVE: To establish an HPLC method for the accurate determination of gliquidone tablets and to solve the problem that the content determination method in the current quality standard is not exclusive and the preparation method of the test solution is not reasonable. Methods: Degradation impurities were analyzed by UPLC-MS. Simultaneous positive and negative ions scanning and ion-scan mode were adopted. The column was ACQUITY UPLC BEH C18 column (50 mm × 2.1 mm, 1.7 μm) with mobile phase of water Adjust pH to 3.5) (A) - acetonitrile (B) gradient. The contents of gliquidone tablets were determined by HPLC. The Agilent Zorbax SB-C18 column (150 mm × 4.6 mm, 5 μm) was used. The mobile phase consisted of water (adjusted to pH 3.5 with formic acid) -acetonitrile (37.5: 62.5). The detection wavelength was 230 nm, the column temperature was 30 ℃, the flow rate was 1.0 ml · min-1 and the injection volume was 20μl. Results: Gliquidone had a good linear relationship with peak area in the range of 60.200-140.400μg · ml-1 (r = 0.999 5), with an average recovery of 98.60% and a RSD of 0.6% (n = 9). Conclusion: The method is accurate, reliable, specific and reproducible. It can be used for the determination of content and content uniformity of gliquidone tablets.