通过氧化偶合和重氮偶合反应测定药物制剂中的米诺环素。

Determination of minocycline by oxidative coupling and diazocoupling reactions in pharmaceutical formulations.

作者信息

Prasad Adapa V S S, Lakshmi Chilukuri S R, Sastry Chilukuri S P, Uppuleti Viplava P

机构信息

Foods and Drugs Laboratories, School of Chemistry, Visakhapatnam 530 003, India.

出版信息

J Pharm Biomed Anal. 2002 Oct 15;30(3):491-8. doi: 10.1016/s0731-7085(02)00215-7.

DOI:10.1016/s0731-7085(02)00215-7

PMID:12367673

Abstract

Simple and sensitive spectrophotometric methods (M(1)-M(4)) by the application of oxidative coupling and diazocoupling reactions for the assay of minocycline (MC) in pure form and pharmaceutical formulations have been described. Methods M(1) and M(2) involve the oxidative coupling reactions of MC with 3-methyl-2-benzothiozolinone hydrazone (MBTH) (method M(1), lambda(max) 440 nm) or 4-aminophenazone (4-AP) (method M(2), lambda(max) 520 nm) in the presence of periodate. Methods M(3) and M(4) are based on the formation of diazocoupling products of MC with diazotised p-nitroaniline (DPNA) (method M(3), lambda(max) 420 nm) or diazotised sulfanilic acid (DSAC) (method M(4), lambda(max) 420 nm). Regression analysis of Beer's law plot showed good correlation in the concentration range of 8-48, 20-120, 4-20 and 8-40 microg ml(-1) for methods A, B, C and D, respectively. The molar absorptivities fell within the range of 2.23 x 10(3)-1.51 x 10(4) l mol(-1) cm(-1). The recoveries range from 99.02 to 100.61%.

摘要

本文描述了通过氧化偶合和重氮偶合反应测定纯米诺环素（MC）及药物制剂中米诺环素的简单灵敏的分光光度法（方法M(1)-M(4)）。方法M(1)和M(2)涉及在高碘酸盐存在下，MC与3-甲基-2-苯并噻唑啉酮腙（MBTH）（方法M(1)，最大吸收波长440 nm）或4-氨基苯乙酮（4-AP）（方法M(2)，最大吸收波长520 nm）的氧化偶合反应。方法M(3)和M(4)基于MC与重氮化对硝基苯胺（DPNA）（方法M(3)，最大吸收波长420 nm）或重氮化磺胺酸（DSAC）（方法M(4)，最大吸收波长420 nm）形成重氮偶合产物。比尔定律曲线的回归分析表明，方法A、B、C和D在浓度范围分别为8 - 48、20 - 120、4 - 20和8 - 40 μg ml⁻¹时具有良好的相关性。摩尔吸光率在2.23×10³ - 1.51×10⁴ l mol⁻¹ cm⁻¹范围内。回收率在99.02%至100.61%之间。