摘要
目的:建立测定缬沙坦氨氯地平片中有关物质的HPLC法。方法:采用KromasilC18(250mm×4.6mm,5μm)色谱柱,流动相为20mmol·L-1庚烷磺酸钠溶液(含0.7%三乙胺,用磷酸调pH值至3.0)(A)-乙腈(B),梯度洗脱;柱温35℃;流速1.0mL·min-1;进样量20μL;检测波长237nm。结果:缬沙坦、氨氯地平和各有关物质的分离符合要求,缬沙坦的已知杂质B、杂质C和氨氯地平的已知杂质D的线性范围及相关系数分别为:0.161~16.103μg·mL-1(n=9,r=1.0000),0.080-8.019μg·mL-1(n=9,r=1.0000),0.063~2.110μg·mL-1(n=9,r=0.9998);检测限分别为0.41,0.72,0.88ng;定量限分别为1.36,2.41,2.94ng;回收率分别为99.8%(n=9,RSD为3.59%),98.6%(n=9,RSD为1.02%),108.5%(n=9,RSD=3.61%)。结论:缬沙坦氨氯地平片中主成分与已知杂质及其他有关物质均分离良好,该方法简单、准确、可靠、专属性强,可用于缬沙坦氨氯地平片有关物质的考察。
Objective : To establish an HPLC method for the determination of the relative substances in val- sartan and amlodipine tablets. Methods: The separation was carried out on a Kromasil C18 column (250 mm ×4.6 mm, 5μm) with gradient elution. The mobile phase consisted of 20 retool. L-1 sodium heptanesulfonate solution, in which 7.0 mL of triethylamine was added into 1 000 mL of water, and pH was adjusted to 3.0 with phosphoric acid (A)-acetonitrile (B). The program was follows: 0 - 10 min, 37% B; 10 - 30 min, 37% B→70% B; 30 45 min, 70% B; 45 -50 min, 70% B→37% B; 50 -60 rain, 37% B. Column temperature was set at 35 ℃. The flow rate was at 1.0 mL. min-1 and the injection volume was 20 μL. The detection wavelength was set at 237 nm. Results: The separation of valsartan, amlodipine and the relative substances met the requirements. The linear ran- ges of the related substances B and C of valsartan, and the related substance D of amlodipine were 0. 161 - 16. 103 μg-mL-1(n=9, r=1.000), 0. 080 - 8. 019 μg.mL-1(n =9, r =1.000) 0.063 -2. 11 μg.mL-1(n =9,r = 0.9998). The LODs were0.41, 0.72 and0.88 ng, and LOQs were 1.36, 2.41 and 2.94ng, respectively. The recoveries were 99.8% (n=9, RSD=3.59%), 98.6% (n=9, RSD=1.02%) and 108.5% (n=9, RSD = 3.61% ). Conclusion: The related substances B and C of valsartan and D of amlodipine or other unknown impuri- ties can be well separated from main ingredients of valsartan and amlodipine. The method is simple, accurate, reli- able and specific. It can be used to determinate the related substances of valsartan and amlodipine tablets.
出处
《中国新药杂志》
CAS
CSCD
北大核心
2013年第19期2323-2327,2331,共6页
Chinese Journal of New Drugs