高效液相色谱法检测维格列汀对映异构体的含量
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摘要
目的:建立R-维格列汀的检测方法。方法:采用高效液相色谱法,色谱柱采用CHIRALPAK R IC手性柱(4.6mm×250mm,5μm),流动相为乙醇-二乙胺(100∶0.1),柱温:25℃,流速为0.5mL/min;检测波长为210nm;进样量10μL。结果:R-维格列汀的检测限和定量限分别为0.309μg/mL和1.236μg/mL,R-维格列汀在0.5～10.0μg/mL范围内线性关系良好(r=0.9996);平均回收率为100.12%(RSD=0.80%);4批样品检测结果表明,其R-维格列汀含量均低于检测限。结论:本方法操作简便、快捷,结果准确、可靠,可用于R-维格列汀的含量控制。
Objective:To establish a HPLC method for determining the enantiomer content of vildagliptin(R-vildagliptin).Methods:HPLC method was adopted. The determination was performed on chiral column of CHIRALPAKRIC(4.6 mm×250 mm, 5μm)with mobile phase consisted of ethanol-diethylamine(100∶0.1) at flow rate of 0.5 mL/min. The detection wavelength was 210 nm and the injection sample volume was 10μL. Results:The limit of detection and quantitation of R-vildagliptin were 0.309μg/mL and 1.236μg/mL, respectively.The linear range of R-vildagliptin was 0.5～10.0μg/mL(r=0.9996)with an average recovery of 100.12%(RSD=0.80%). The contents of R-vildagliptin in 4 batches of samples were below the limit of detection. Conclusion:The method is simple,rapid,accurate and reliable,and it is applicable for the quality control of R-vildagliptin.
Objective:To establish a HPLC method for determining the enantiomer content of vildagliptin(R-vildagliptin).Methods:HPLC method was adopted. The determination was performed on chiral column of CHIRALPAKRIC(4.6 mm×250 mm, 5μm)with mobile phase consisted of ethanol-diethylamine(100∶0.1) at flow rate of 0.5 mL/min. The detection wavelength was 210 nm and the injection sample volume was 10μL. Results:The limit of detection and quantitation of R-vildagliptin were 0.309μg/mL and 1.236μg/mL, respectively.The linear range of R-vildagliptin was 0.5～10.0μg/mL(r=0.9996)with an average recovery of 100.12%(RSD=0.80%). The contents of R-vildagliptin in 4 batches of samples were below the limit of detection. Conclusion:The method is simple,rapid,accurate and reliable,and it is applicable for the quality control of R-vildagliptin.
引文
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[2]苏永,吕丽芳,李全忠,等.维格列汀与α-糖苷酶抑制剂治疗2型糖尿病的随机对照临床试验[J].中国新药杂志,2014,23(22):2655.
[3]李彦,张先祥,罗涌,等.维格列汀对新诊断超重2型糖尿病患者炎症因子的影响研究[J].中国药房,2013,24(26):2449.
[4]BrandtI,Joossens J,Chen X,et al.Inhibition of dipeptidyl-peptidase IV catalyzed peptide truncation by Vildagliptin((2S)-{[(3-hydroxyadamantan-1-yl)amino]acetyl}-pyrrolidine-2-carbonitrile)[J].Biochemical Pharmacology,2005,70(1):134-143.
[5]E.B.威尔豪尔.N-取代2-氰基吡咯烷类化合物[P].中国专利:99814202.6,2002-01-02.
[6]Anonym.SCIENTIFIC DISCUSSION.http://www.ema.europa.eu/docs/en_GB/document_library/EPAR_-_Scientific_Discussion/human/000771/WC500020330.pdf[2015-12-06].
[7]国家食品药品监督管理局.JX20100243维格列汀片进口药品注册标准[S].2011.