Investigation of electrochemical behavior of anisomycin on gold electrode followed by HPLC–MS/MS analysis

Abstract

Anisomycin is an immunosuppressant in low doses (b0.1 μM) with possible application in treatment of some autoimmune diseases and in inhibiting transplantation rejection. Anisomycin suppresses malignant tumor cell growth and affects memory. For the first time it was the subject of the electrochemical investigations by cyclic voltammetry and square wave voltammetry on gold electrode in 0.05 M NaHCO 3 using its electrochemical activity. The cyclic voltammetry experiments at different sweep rates show that electrochemical process is irreversible and diffusion controlled. Based on square wave voltammetry measurements, the calculated values of LOD and LOQ were 1 and 4 nM (in the absence of biological fluid), as well as 2 and 6 nM (in the presence of spiked urine) indicating the high sensitivity of the proposed electroanalytical method. High performance liquid chromatography-tandem mass spectrometry was a reference method for quantification of anisomycin and served for structural identification of its hydrolysis product (deacetylanisomycin).

Contribution to the Recent Advances in Electrochemical Analysis of Pharmaceuticals

“…The electrochemical activity of anisomycin was investigated on gold electrode using cyclic voltammetry in 0.05 M NaHCO 3 [ 12 ]. Square wave voltammetry was applied for quantitative determination of the drug and in spiked urine samples, followed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).…”

“…In the fi rst 2 h, the amount of anisomycin decreases while the amount of hydrolysis product increases. After that, the amounts of both anisomycin and the hydrolysis product decrease and by the end of Step size 5 mV, pulse size 100 mV, frequency 2 Hz and scan rate 10 mV s −1 , accumulation time 200 ms at 0.0 V. Inset : linear dependency of anodic peak currents vs. concentration of anisomycin (Reproduced with a permission from Elsevier) [ 12 ] the experiment (4 h) their presence was neglectable. This confi rms that after 2 h the electrooxidation products cause the apparent increase of anodic currents in Fig.…”

“…Cardiovascular drugs belong also to the most prescribed medications nowadays since various cardiovascular diseases are predominant in developed countries worldwide. In this group the most [ 12 ] second-generation dihydropyridine derivatives, it has greater selectivity for the vascular smooth muscle than myocardial tissue and therefore their main effect is vasodilatation. Amlodipine is used alone or in combination with other medicines for the treatment of chronic stable angina, certain types of vasospastic angina, and in the management of mild-to-moderate essential hypertension.…”

“…Fig. 2.15 Cyclic voltammogram of Au electrode using 0.05 M NaHCO 3 ( dashed line ) and with 0.037 nM anisomycin, ( a ) 1. and 20. scan, scan rate: 50 mV s −1 , ( b ) for scan rates: 20, 40, 60, 80, 100, 120, and 140 mV s −1 ,( c) plot of peak current vs. v 1/2 , ( d ) plot of peak potential shift vs. ln of scan rates (Reproduced with a permission from Elsevier)[ 12 ] …”

Determination of anisomycin in tissues and serum by LC-MS/MS: application to pharmacokinetic and distribution studies in rats

“…In our previous study, LC-MS/MS method was used as a comparative method for investigation of anisomycin electrochemical degradation in standard solution and in urine. 27 The aim of this work was to develop the sample preparation method for anisomycin determination in various tissues (brain, spleen, heart, femoral muscle, kidney, liver) and serum as well as to determine its in vivo pharmacokinetics and tissue distribution in rats.…”