RP-HPLC法测定卡博替尼原料药中卡博替尼的含量
|
摘要
目的:建立测定卡博替尼原料药中卡博替尼含量的方法。方法:采用反相高效液相色谱法。色谱柱为Inertsil ODS-SP C_(18),流动相为乙腈-0.02 mol/L乙酸铵缓冲溶液(p H 5.2)(52∶48,V/V),流速为1.0 m L/min,检测波长为241 nm,柱温为38℃,进样量为20μL。结果:卡博替尼检测质量浓度线性范围为9.88~49.40μg/m L(r=0.999 9);定量限为11.46 ng,检测限为3.36 ng;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率为98.5~101.7%(RSD=1.2%,n=9)。结论:该方法操作简便、结果准确,可用于卡博替尼原料药中卡博替尼的含量测定。
OBJECTIVE:To establish a method for the content determination of cabozantinib in its raw material. METHODS:RP-HPLC method was adopted. The determination was performed on Inertsil ODS-SP C_(18) column with mobile phase consisted of acetonitrile-0.02 mol/L ammonium acetate buffer(p H 5.2,52 ∶ 48,V/V)at the flow rate of 1.0 m L/min. Detection wavelength was set at 241 nm,the column temperature was 38 ℃,and sample size was 20 μL. RESULTS:The linear range of cabozantinib were9.88-49.40 μg/m L(r=0.999 9). The limit of quantitation was 11.46 ng,and the limit of detection was 3.36 ng. The RSDs of precision,stability,repeatability tests were all lower than 2.0%;recoveries were 98.5%-101.7%(RSD=1.2%,n=9). CONCLUSIONS:The method is simple,accurate and suitable for the content determination of cabozantinib in its raw material.
OBJECTIVE:To establish a method for the content determination of cabozantinib in its raw material. METHODS:RP-HPLC method was adopted. The determination was performed on Inertsil ODS-SP C_(18) column with mobile phase consisted of acetonitrile-0.02 mol/L ammonium acetate buffer(p H 5.2,52 ∶ 48,V/V)at the flow rate of 1.0 m L/min. Detection wavelength was set at 241 nm,the column temperature was 38 ℃,and sample size was 20 μL. RESULTS:The linear range of cabozantinib were9.88-49.40 μg/m L(r=0.999 9). The limit of quantitation was 11.46 ng,and the limit of detection was 3.36 ng. The RSDs of precision,stability,repeatability tests were all lower than 2.0%;recoveries were 98.5%-101.7%(RSD=1.2%,n=9). CONCLUSIONS:The method is simple,accurate and suitable for the content determination of cabozantinib in its raw material.
引文
[1]Bowles DW,Kessler ER,Jimeno A.Multitargeted tyrosine kinase inhibitors in clinical development:focus on XL-184(cabozantinib)[J].Drugs Today:Barc,2011,47(11):857-868.
[2]张秀颖,刘尧,白秋江,等.新型分子靶向抗癌药物卡博替尼[J].医药导报,2013,32(11):1468-1470.
[3]夏训明.美国FDA批准Cometriq(cabozantinib)治疗甲状腺髓样癌[J].广东药学院学报,2012,28(6):627.
[4]陈惠玲,张志叶,杨彦彪.治疗转移性甲状腺髓样癌的新药:Cabozantinib[J].中国药房,2014,25(29):2766-2769.
[5]郑希元,姜汉杰,蒲小平.抗甲状腺髓样癌新药卡博替尼[J].中国新药杂志,2013,22(17):1990-1993.
[6]吕娟丽,刘洋,孙慧萍.甲状腺髓样癌治疗新药Cabozantinib苹果酸盐[J].中国临床药学杂志,2014,23(1):28-62.
[7]赵锐,张喜全,孟庆义.以c-Met为靶点的小分子酪氨酸激酶抑制剂的研究进展[J].药物与临床研究,2012,20(6):519-522.
[2]张秀颖,刘尧,白秋江,等.新型分子靶向抗癌药物卡博替尼[J].医药导报,2013,32(11):1468-1470.
[3]夏训明.美国FDA批准Cometriq(cabozantinib)治疗甲状腺髓样癌[J].广东药学院学报,2012,28(6):627.
[4]陈惠玲,张志叶,杨彦彪.治疗转移性甲状腺髓样癌的新药:Cabozantinib[J].中国药房,2014,25(29):2766-2769.
[5]郑希元,姜汉杰,蒲小平.抗甲状腺髓样癌新药卡博替尼[J].中国新药杂志,2013,22(17):1990-1993.
[6]吕娟丽,刘洋,孙慧萍.甲状腺髓样癌治疗新药Cabozantinib苹果酸盐[J].中国临床药学杂志,2014,23(1):28-62.
[7]赵锐,张喜全,孟庆义.以c-Met为靶点的小分子酪氨酸激酶抑制剂的研究进展[J].药物与临床研究,2012,20(6):519-522.