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分光光度法测定麦考酚酸酯与其两种π受体的荷移络合物。

Spectrophotometric Determination of Mycophenolate Mofetil as Its Charge-Transfer Complexes with Two π-Acceptors.

机构信息

Department of Chemistry, University of Mysore, Manasagangotri, Mysore 570 006, India.

出版信息

J Anal Methods Chem. 2012;2012:875942. doi: 10.1155/2012/875942. Epub 2012 Mar 26.

Abstract

Two simple, selective, and rapid spectrophotometric methods are described for the determination of mycophenolate mofetil (MPM) in pure form and in tablets. Both methods are based on charge-transfer complexation reaction of MPM with p-chloranilic acid (p-CA) or 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) in dioxane-acetonitrile medium resulting in coloured product measurable at 520 nm (p-CA) or 580 nm (DDQ). Beer's law is obeyed over the concentration ranges of 40-400 and 12-120 μg mL(-1) MPM for p-CA and DDQ, respectively, with correlation coefficients (r) of 0.9995 and 0.9947. The apparent molar absorptivity values are calculated to be 1.06 × 10(3) and 3.87 × 10(3) L mol(-1) cm(-1), respectively, and the corresponding Sandell's sensitivities are 0.4106 and 0.1119 μg cm(-1). The limits of detection (LOD) and quantification (LOQ) are also reported for both methods. The described methods were successfully applied to the determination of MPM in tablets. Statistical comparison of the results with those of the reference method showed excellent agreement. No interference was observed from the common excipients present in tablets. Both methods were validated statistically for accuracy and precision. The accuracy and reliability of the methods were further ascertained by recovery studies via standard addition procedure.

摘要

两种简单、选择性和快速的分光光度法被描述用于测定霉酚酸酯(MPM)的纯品和片剂。两种方法均基于 MPM 与对氯邻苯二甲酸(p-CA)或 2,3-二氯-5,6-二氰基-1,4-苯醌(DDQ)在二氧六环-乙腈介质中的电荷转移络合反应,生成可在 520nm(p-CA)或 580nm(DDQ)处测量的有色产物。对于 p-CA 和 DDQ,比尔定律在 40-400 和 12-120μg·mL(-1)MPM 的浓度范围内得到遵守,相关系数(r)分别为 0.9995 和 0.9947。表观摩尔吸光率值分别计算为 1.06×10(3)和 3.87×10(3)L·mol(-1)·cm(-1),相应的桑德尔灵敏度分别为 0.4106 和 0.1119μg·cm(-1)。还报道了两种方法的检测限(LOD)和定量限(LOQ)。所描述的方法成功地应用于片剂中 MPM 的测定。与参考方法的结果进行统计比较显示出极好的一致性。片剂中常见赋形剂没有干扰。两种方法均从准确度和精密度方面进行了统计学验证。通过标准加入程序的回收研究进一步确定了方法的准确性和可靠性。

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