Objective: To establish a method for determining the absolute contents of candesartan cilexetil and amlodipine besylate in candesartan cilexetil and amlodipine tablets by qNMR. Methods: The chemical shift δ 5.51 of candesartan cilexetil and δ 5.31 of amlodipine besylate were used as the quantitative peaks. δ 6.27 of maleic acid was the quantitative peak of internal standard. DMSO-d6 was used as the solvent. Results: The method was highly specific and the solvent peak, water peak and excipient peaks did not interfere with the quantitative peaks. Candesartan cilexetil showed a good linear relationship in the concentration range of 1.580 0- 9.480 2 mg·mL-1, r=1.000, RSDs of precision, repeatability and stability were 0.070%, 1.7% and 0.68%, respectively. The recoveries of low, medium and high concentration spiked were 98.1%-99.2%. The linear range of amlodipine besylate was 0.983 9-5.903 6 mg·mL-1 (r=0.999 9). The RSDs of precision, repeatability and stability were 0.050%, 1.8% and 0.79%, respectively. The recovery of amlodipine besylate was 99.1%-102.0%. This method was used to test two batches of reference preparations and one batch of sample from different sources. The results showed that the content of candesatan cilexetil was between 98.10% to 98.75%, and that of amlldipine besylate was between 98.98% to 99.60%. Conclusion: This method is rapid and accurate and it is not necessary to use a single component reference substance. This method provides a new method to determine the content to candesartan cilexetil and amlodipine tablets.
ZHANG Zhong-ling, WU Hong-Hai, CHEN Zhong-kui, WENG Qin-jie
. Determination of absolute contents of candesartan cilexetil and amlodipine besylate in candesartan cilexetil and amlodipine tablets by quantitative nuclear magnetic resonance[J]. Chinese Journal of Pharmaceutical Analysis, 2024
, 44(3)
: 373
-379
.
DOI: 10.16155/j.0254-1793.2024.03.01
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