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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nifdc.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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UHPLC-MS/MS法测定比格犬血浆中硝苯地平的浓度

Determination of nifedipine in Beagles plasma by UHPLC-MS/MS

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出版年·卷·期(页码):2014,34 (1):0-0
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立UHPLC-MS/MS法测定硝苯地平缓释片在比格犬血浆中的药物浓度。方法:血浆经乙醚-正己烷(2:1)提取,以地西泮为内标,采用UHPLC-MS/MS方法测定6只比格犬口服硝苯地平缓释片20 mg后血浆中的药物浓度。UHPLC条件:采用Shim-pack XR-ODS色谱柱(75 mm×3.0 mm,2.2 μm),以甲醇(B)-0.05%甲酸水(A)为流动相,洗脱梯度(0~2.00 min,80%B→95%B;2.01~2.20 min,95%B;2.21~3.50 min,80%B),流速0.4 mL·min-1,柱温40℃,分析时间总计3.50 min,进样量5 μL;条件:硝苯地平:m/z347.0→m/z315.0,DP为58 V,CE为10 V,CXP为21 V;地西泮(内标):m/z285.0→m/z193.1,DP为80 V,CE为43 V,CXP为20 V。结果:硝苯地平在浓度为0.15~50.00 ng·mL-1范围内线性关系良好(r=0.9983),日内精密度RSD(n=6)≤6.6%,日间精密度RSD(n=6)≤13.8%,绝对回收率(n=6)为63.1%~68.3%,基质效应(n=6)RSD≤7.5%。6只比格犬口服硝苯地平缓释片20 mg后的主要药动学参数Tmax为(4.58±1.39)h,Cmax为(30.53±7.38)ng·mL-1t1/2为(8.69±3.42)h,AUC0-t为(185.9±113.3)ng·h·mL-1,AUC0-∞为(188.8±113.6)ng·h·mL-1结论:本方法简单、快速、灵敏,重现性好,可用于测定硝苯地平缓释片的血药浓度并进行药动学评价。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To develop a UHPLC-MS/MS method for the determination of the drug concentration in Beagles plasma after oral administration of nifedipine sustained-release tablets. Methods: Diazepam was used as the internal standard.The concentration of nifedipine in the six Beagles plasma was determined by UHPLC-MS/MS after oral administration of 20 mg of nifedipine sustained-release tablets.Nifedipine and internal standard were separated by Shim-pack XR-ODS(75 mm×3.0 mm,2.2 μm)and extracted from plasma by ethyl ether-n-hexane(2: 1).Mobile phase was methanol-0.05% formic acid in water with gradient elution(0-2.00 min,80%B→95%B;2.01-2.20 min,95%B;2.21-3.50 min,80%B),the flow rate was 0.4 mL·min-1 with the column temperature of 40℃,the total analysis time was 3.50 min and the inject volume was 5 μL;MS:nifedipine:m/z 347.0→m/z 315.0,DP:58 V,CE:10 V,CXP:21 V;diazepam(internal standard):m/z 285.0→m/z 193.1,DP:80 V,CE:43 V,CXP:20 V.Results: The linear range of nifedipine in the plasma was 0.15-50.00 ng·mL-1(r=0.9983),the intra-day and inter-day precisions were lower than 6.6%(n=6)and 13.8%(n=6),the recovery(n=6)was 63.1%-68.3% and the RSD(n=6)of matrix effect was lower than 7.5%.The main pharmacokinetic parameters of nifedipine in Beagles were as follows:Tmax was(4.58±1.39)h,Cmax was(30.53±7.38)ng·mL-1,t1/2 was(8.69±3.42)h,AUC0-t was(185.9±113.3)ng·h·mL-1,and AUC0-∞ was(188.8±113.6)ng·h·mL-1. Conclusion: The method is simple,fast,sensitive and reproducible for the determination of nifedipine in nifedipine sustained-release tablets and in the pharmacokinetic assays.

-----参考文献:---------------------------------------------------------------------------------------

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