高效液相色谱法测定缬沙坦氨氯地平片中的有关物质

Determination of related substances in valsartan and amlodipine tablets by HPLC

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.