一阶导数同步荧光法同时测定药物制剂中的乙酰水杨酸和咖啡因
Simultaneous determination of acetylsalicylic acid and caffeine in pharmaceutical formulation by first derivative synchronous fluorimetric method.
作者信息
Karim Mohammad Mainul, Jeon Chi Wan, Lee Hyun Sook, Alam Seikh Mafiz, Lee Sang Hak, Choi Jong Ha, Jin Seung Oh, Das Ajoy Kumar
机构信息
Department of Chemistry, Kyungpook National University, Taegu 702-701, Republic of Korea.
出版信息
J Fluoresc. 2006 Sep;16(5):713-21. doi: 10.1007/s10895-006-0115-7. Epub 2006 Sep 2.
A sensitive, rapid, and specific assay has been developed for the simultaneous determination of acetylsalicylic acid and caffeine in commercial tablets based on their natural fluorescence. The mixture of these drugs was resolved by first derivative synchronous fluorimetric technique using two scans. At Deltalambda=106 nm, using first derivative synchronous scanning, only acetylsalicylic acid yields a detectable signal at 316 nm (peak to zero method) which is unaffected by caffeine. At Deltalambda=30 nm, the signal of caffeine at 288 nm (peak to zero method) is not affected by acetylsalicylic acid. The range of application is between 0.021 and 41.62 microg ml(-1) (correlation coefficient, R=0.9995) for acetylsalicylic acid and between 0.4486 and 44.86 microg ml(-1) (correlation coefficient, R=0.99786) for caffeine. The recovery range of 98.40-102% for acetylsalicylic acid and 90-100.5% for caffeine from their synthetic mixture was reported. Overall recovery of both compounds about 97-99% for acetylsalicylic acid and 97-98% for caffeine was obtained from real sample analysis. The detection limits are 0.0013 microg ml(-1) and 0.0306 microg ml(-1) for acetylsalicylic acid and caffeine, respectively. The relative standard deviation (n=10) for 20 microg ml(-1) of acetylsalicylic acid is 2.75% and for 2.2 microg ml(-1)of caffeine is 1.7%.
基于乙酰水杨酸和咖啡因的天然荧光，开发了一种灵敏、快速且特异的方法，用于同时测定市售片剂中的乙酰水杨酸和咖啡因。采用一阶导数同步荧光技术，通过两次扫描来解析这两种药物的混合物。在Δλ = 106 nm时，使用一阶导数同步扫描，仅乙酰水杨酸在316 nm处产生可检测信号（峰-零法），该信号不受咖啡因影响。在Δλ = 30 nm时，咖啡因在288 nm处的信号（峰-零法）不受乙酰水杨酸影响。乙酰水杨酸的应用范围为0.021至41.62 μg ml⁻¹（相关系数，R = 0.9995），咖啡因的应用范围为0.4486至44.86 μg ml⁻¹（相关系数，R = 0.99786）。据报道，从合成混合物中回收乙酰水杨酸的范围为98.40 - 102%，回收咖啡因的范围为90 - 100.5%。通过实际样品分析，两种化合物的总体回收率为：乙酰水杨酸约97 - 99%，咖啡因为97 - 98%。乙酰水杨酸和咖啡因的检测限分别为0.0013 μg ml⁻¹和0.0306 μg ml⁻¹。20 μg ml⁻¹乙酰水杨酸的相对标准偏差（n = 10）为2.75%，2.2 μg ml⁻¹咖啡因的相对标准偏差为1.7%。
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