α_1-酸性糖蛋白手性固定相测定埃索美拉唑钠中对映异构体杂质的含量
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摘要
目的:采用α_1-酸性糖蛋白手性固定相高效液相色谱法测定埃索美拉唑钠原料药中对映异构体杂质的含量。方法:采用CHIRAL-AGP手性固定相柱(150 mm×4 mm,5μm);检测波长:302 nm;流动相:磷酸盐(0. 01 mol·L~(-1),pH 6. 0)-乙腈(17∶3);流速:0. 8 ml·min~(-1);柱温:25℃;进样量:20μl。结果:埃索美拉唑钠与其对映异构体能够完全分离,对映异构体在0. 08～0. 40μg·ml~(-1)范围内线性关系良好(r=0. 999 8),加样回收率为100. 4%(RSD=1. 02%,n=9)。结论:该方法快速、准确,可用于埃索美拉唑钠原料药中对映异构体杂质含量的测定。
Objective: To determine the content of enantiomer impurity in esomeprazole sodium by α_1-acidglycoprotein chiral column. Methods: A CHIRAL-AGP chiral stationary phase column (150 mm × 4 mm,5 μm) was used,the detection wavelength was302 nm,the mobile phase was phosphate (0. 01 mol·L~(-1),pH 6. 0)-acetonitrile (17 ∶ 3),the flow rate was 0. 8 ml·min~(-1),the column temperature was 25 ℃ and the injection volume was 20 μl. Results: Esomeprazole sodium and its enantiomer impurity could be separated completely. The calibration curve was linear within the range of 0. 08-0. 40 μg·ml~(-1) (r = 0. 999 8). The recovery was 100. 4% (RSD = 1. 02%,n = 9). Conclusion: The present method is rapid and simple,and can be used to determine the content of enantiomer impurity in esomeprazole sodium.
Objective: To determine the content of enantiomer impurity in esomeprazole sodium by α_1-acidglycoprotein chiral column. Methods: A CHIRAL-AGP chiral stationary phase column (150 mm × 4 mm,5 μm) was used,the detection wavelength was302 nm,the mobile phase was phosphate (0. 01 mol·L~(-1),pH 6. 0)-acetonitrile (17 ∶ 3),the flow rate was 0. 8 ml·min~(-1),the column temperature was 25 ℃ and the injection volume was 20 μl. Results: Esomeprazole sodium and its enantiomer impurity could be separated completely. The calibration curve was linear within the range of 0. 08-0. 40 μg·ml~(-1) (r = 0. 999 8). The recovery was 100. 4% (RSD = 1. 02%,n = 9). Conclusion: The present method is rapid and simple,and can be used to determine the content of enantiomer impurity in esomeprazole sodium.
引文
1 Dent J.Review article:pharmacology of esomeprazole and comparisons with omeprazole[J].Aliment Pharmacol Ther,2003,17:5-9
2 Lind T,Rydberg L,Kylebck A,et al.Esomeprazole provides improved acid control vs.omeprazole In patients with symptoms of gastro-oesophageal reflux disease[J].Aliment Pharmacol Ther,2000,14(7):861-867
3 Sandstr9m M,Davidson G,Tolia V,et al.Phase I,multicenter,randomized,open-label study evaluating the pharmacokinetics and safety profile of repeated once-daily doses of intravenous esomeprazole in children 0 to 17 years of age[J].Clin Ther,2012,34(8):1828-1838
4 Vyas S,Patel A,Ladva KD,et al.Development and validation of a stability indicating method for the enantioselective estimation of omeprazole enantiomers in the enteric-coated formulations by high-performance liquid chromatography[J].J Pharm Bioallied Sci,2011,3(2):310-314
5卢定强,李衍亮,涂清波,等.高效液相色谱直链淀粉手性固定相拆分奥美拉唑对映体[J].2010,27(1):66-69
6邵红.键合纤维素手性固定相拆分奥美拉唑对映体[J].中国医药指南,2014,12(8):39-40
7 Ma Z,Zhang L,Lin L,et al.Enantioseparation of rabeprazole and omeprazole by nonaqueous capillary electrophoresis with an ephedrine-based ionic liquid as the chiral selector[J].Biomed Chromatogr,2010,24(12):1332-1337
8周长民,关瑾,任丽艳,等.柱前衍生化高效液相色谱法分离分析奥美拉唑对映体[J].2012,10(5):353-355
9中国药典[S].2015年版.二部.1412
2 Lind T,Rydberg L,Kylebck A,et al.Esomeprazole provides improved acid control vs.omeprazole In patients with symptoms of gastro-oesophageal reflux disease[J].Aliment Pharmacol Ther,2000,14(7):861-867
3 Sandstr9m M,Davidson G,Tolia V,et al.Phase I,multicenter,randomized,open-label study evaluating the pharmacokinetics and safety profile of repeated once-daily doses of intravenous esomeprazole in children 0 to 17 years of age[J].Clin Ther,2012,34(8):1828-1838
4 Vyas S,Patel A,Ladva KD,et al.Development and validation of a stability indicating method for the enantioselective estimation of omeprazole enantiomers in the enteric-coated formulations by high-performance liquid chromatography[J].J Pharm Bioallied Sci,2011,3(2):310-314
5卢定强,李衍亮,涂清波,等.高效液相色谱直链淀粉手性固定相拆分奥美拉唑对映体[J].2010,27(1):66-69
6邵红.键合纤维素手性固定相拆分奥美拉唑对映体[J].中国医药指南,2014,12(8):39-40
7 Ma Z,Zhang L,Lin L,et al.Enantioseparation of rabeprazole and omeprazole by nonaqueous capillary electrophoresis with an ephedrine-based ionic liquid as the chiral selector[J].Biomed Chromatogr,2010,24(12):1332-1337
8周长民,关瑾,任丽艳,等.柱前衍生化高效液相色谱法分离分析奥美拉唑对映体[J].2012,10(5):353-355
9中国药典[S].2015年版.二部.1412