正相高效液相色谱法测定注射用右旋兰索拉唑中左旋异构体的含量
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摘要
将注射用右旋兰索拉唑粉末用甲醇溶解配制成5.00mg·L~(-1)的样品溶液,在以下条件下进行色谱分析:采用Chiralpak ID手性色谱柱(4.6 mm×250 mm,5μm)为固定相,柱温为35℃,流动相为正己烷-异丙醇-冰乙酸(70+30+0.2)混合液,流量为0.6mL·min~(-1),二极管阵列检测器,检测波长为285nm。结果表明:左旋兰拉唑的质量浓度在0.48～4.81mg·L~(-1)内与其峰面积呈线性关系,检出限(3S/N)为2.4×10~(-3) mg·L~(-1),测定下限(10S/N)为4.8×10~(-3) mg·L~(-1)。加标回收率在97.5%～103%之间,测定值的相对标准偏差(n=6)小于1.6%。
The(R)-lansoprazole powder for injection was dissolved in methanol to prepare a 5.00 mg·L~(-1) sample solution,and chromatographic analysis was carried out under the following conditions:Chiralpak ID chiral column(4.6 mm×250 mm,5μm)was used as stationary phase,the column temperature was 35 ℃,the mobile phase was a mixture of n-hexane,isopropanol and glacial acetic acid(70+30+0.2),the flow rate was 0.6 mL·min~(-1),and the diode array detector was used for detection at the wavelength of 285 nm.The results showed that,linear relationship was found between peak area and mass concentration of(S)-lansoprazole in the range of 0.48-4.81 mg·L~(-1),the detection limit(3 S/N)was 2.4×10~(-3) mg·L~(-1),and the lower limit of determination(10 S/N)was 4.8×10~(-3) mg·L~(-1).Values of recovery obtained by standard addition method were in the range of 97.5%-103%,and RSDs(n=6)were less than 1.6%.
The(R)-lansoprazole powder for injection was dissolved in methanol to prepare a 5.00 mg·L~(-1) sample solution,and chromatographic analysis was carried out under the following conditions:Chiralpak ID chiral column(4.6 mm×250 mm,5μm)was used as stationary phase,the column temperature was 35 ℃,the mobile phase was a mixture of n-hexane,isopropanol and glacial acetic acid(70+30+0.2),the flow rate was 0.6 mL·min~(-1),and the diode array detector was used for detection at the wavelength of 285 nm.The results showed that,linear relationship was found between peak area and mass concentration of(S)-lansoprazole in the range of 0.48-4.81 mg·L~(-1),the detection limit(3 S/N)was 2.4×10~(-3) mg·L~(-1),and the lower limit of determination(10 S/N)was 4.8×10~(-3) mg·L~(-1).Values of recovery obtained by standard addition method were in the range of 97.5%-103%,and RSDs(n=6)were less than 1.6%.
引文
[1]刁依娜,杨正兵,蒋学华.注射用兰索拉唑治疗65例十二指肠溃疡伴出血患者的疗效[J].华西药学杂志,2014,29(5):611-612.
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[8]党靖涛,王茜莎,杨威,等.LEW002对动物试验性急性胃溃疡的影响[J].广东化工,2015,42(13):69-72.
[9] SACHS G,SHIN J M,HOWDEN C W.Review article:The clinical pharmacology of proton pump inhibitors[J].Alimentary Pharmacology and Therapeutics,2006,23(s2):2-8.
[10] KUKULKA M,WU J T,PEREZ M C.Pharmacokinetics and safety of dexlansoprazole MR in adolescents with symptomatic GERD[J].Journal of Pediatric Gastroenterology and Nutrition,2012,54(1):41-47.
[11] HERSHCOVICI T,JHA L K,FASS R.Dexlansoprazole MR-A review[J].Annals of Medicine,2011,43(5):366-374.
[12] KATSUKI H,YAGI H,ARIMORI K,et al.Determination of R(+)-and S(-)-lansoprazole using chiral stationary-phase liquid chromatography and their enantioselective pharmacokinetics in humans[J].Pharmaceutical Research,1996,13(4):611-615.
[13]党靖涛.ASKC263的药效学研究[D].广州:广东药学院,2015.
[14]郭俊平.HPLC法测定右旋兰索拉唑控释胶囊中左旋异构体含量[J].药学与临床研究,2014,22(3):228-230.
[15]崔欣,付芳敏,朱槿,等.奥美拉唑、兰索拉唑对映体及相关物质在不同手性柱的分离比较[J].分析化学,2002,30(12):1494-1496.
[2] METZ D C,VAKILY M,DIXIT T,et al.Review article:Dual delayed release formulation of dexlansoprazole MR,a novel approach to overcome the limitations of conventional single release proton pump inhibitor therapy[J].Alimentary Pharmacology&Therapeutics,2009,29(9):928-937.
[3] FASS R,INADOMI J,HAN C,et al.Maintenance of heartburn relief after step-down from twice-daily proton pump inhibitor to once-daily dexlansoprazole modified release[J].Clinical Gastroenterology and Hepatology,2012,10(3):247-253.
[4]侯艳,谭娇梅,乔红群,注射用右旋兰索拉唑的遗传毒性研究[J].华西药学杂志,2017,32(6):595-598.
[5] SUN L N,CAO Y,JIAO H W,et al.Enantioselective determination of(R)-and(S)-lansoprazole in human plasma by chiral liquid chromatography with mass spectrometry and its application to a stereoselective pharmacokinetic study[J].Journal of Separation Science,2015,38(21):3696-3703.
[6] KUKULKA M,NUDURUPATI S,PEREZ M C.Pharmacokinetics and safety of dexlansoprazole MR in pediatric patients with symptomatic gastroesophageal reflux disease[J].Clinical and Experimental Gastroenterology,2014,7:461-471.
[7] FRELINGER A L,LEE R D,MULFORD D J,et al.A randomized,2-period,crossover design study to assess the effects of dexlansoprazole,lansoprazole,esomeprazole,and omeprazole on the steady-state pharmacokinetics and pharmacodynamics of clopidogrel in healthy volunteers[J].Journal of the American College of Cardiology,2012,59(14):1304-1311.
[8]党靖涛,王茜莎,杨威,等.LEW002对动物试验性急性胃溃疡的影响[J].广东化工,2015,42(13):69-72.
[9] SACHS G,SHIN J M,HOWDEN C W.Review article:The clinical pharmacology of proton pump inhibitors[J].Alimentary Pharmacology and Therapeutics,2006,23(s2):2-8.
[10] KUKULKA M,WU J T,PEREZ M C.Pharmacokinetics and safety of dexlansoprazole MR in adolescents with symptomatic GERD[J].Journal of Pediatric Gastroenterology and Nutrition,2012,54(1):41-47.
[11] HERSHCOVICI T,JHA L K,FASS R.Dexlansoprazole MR-A review[J].Annals of Medicine,2011,43(5):366-374.
[12] KATSUKI H,YAGI H,ARIMORI K,et al.Determination of R(+)-and S(-)-lansoprazole using chiral stationary-phase liquid chromatography and their enantioselective pharmacokinetics in humans[J].Pharmaceutical Research,1996,13(4):611-615.
[13]党靖涛.ASKC263的药效学研究[D].广州:广东药学院,2015.
[14]郭俊平.HPLC法测定右旋兰索拉唑控释胶囊中左旋异构体含量[J].药学与临床研究,2014,22(3):228-230.
[15]崔欣,付芳敏,朱槿,等.奥美拉唑、兰索拉唑对映体及相关物质在不同手性柱的分离比较[J].分析化学,2002,30(12):1494-1496.