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. 2022 May 18;12(1):8270.
doi: 10.1038/s41598-022-12506-9.

Simultaneous electrochemical determination of morphine and methadone by using CMK-5 mesoporous carbon and multivariate calibration

Mohammad Mehdi Habibi  1 , Jahan B Ghasemi  2 , Alireza Badiei  1 , Parviz Norouzi  3
Affiliations

Simultaneous electrochemical determination of morphine and methadone by using CMK-5 mesoporous carbon and multivariate calibration

Mohammad Mehdi Habibi et al. Sci Rep. .

Abstract

For the first time, a sensitive electrochemical sensor using a glassy carbon electrode modified with CMK-5 Ordered mesoporous carbon was fabricated for simultaneous analysis of morphine and methadone. Modern electrochemical FFT-SWV techniques and partial least-squares as a multivariable analysis were used in this method. CMK-5 nanostructures were characterized by field emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction analysis, and Raman spectroscopy. Variables such as accumulation time and pH for the proposed sensor were optimized before quantitative analysis. To train the proposed sensor, standard mixtures of morphine (MOR), and methadone (MET) were prepared in the established linear ranges of the analyzes. The results obtained from training samples were used for PLS modeling. The efficiency of the model was determined using test and real matrix samples. The root mean square error of prediction and the squared correlation coefficients (R2p) for MET and MOR were estimated to be 0.00772 and 0.00892 and 0.948 to 0.990, respectively. The recoveries in urine samples were reported to be 97.0 and 105.6% for both MOR and MET, respectively.

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Conflict of interest statement

The authors declare no competing interests.

Figures

Figure 1
Figure 1
Electrochemical reaction of morphine and methadone.
Figure 2
Figure 2
Schematic representation of the simultaneous electrochemical detection of MOR and MET at CMK-5 Mesoporous Carbon Surface by a combination of FFT-SWV with Multivariate Calibration.
Figure 3
Figure 3
Schematic representation of the preparation procedure of CMK-5 mesoporous carbon by the nanocasting strategy using an Al-SBA-15 hard template.
Figure 4
Figure 4
Applied potential waveform during FFT-SWV measurements.
Figure 5
Figure 5
(A) SEM, (B) TEM, (C) EDS spectrum and EDS mapping image of CMK-5.
Figure 6
Figure 6
EIS characterization of GC and GC-CMK-5 electrode in 5.0 mM Fe(CN)6−3/4 containing 0.1 M KCl with the frequency range of 0.1 Hz to 100 kHz at an amplitude of 10 mV.
Figure 7
Figure 7
(A) and (B) Cyclic voltammograms of GC electrode presence of individual MOR, MET. (C) and (D) GC/CMK-5 electrode presence of individual MOR, MET and (E) GC/CMK-5 electrode presence of MOR, MET mixture.
Figure 8
Figure 8
(A) Calibration plot of pH versus potential and (B) optimization plot of pH versus current. (C) Optimization of accumulation time (0–180 s) of 2 µM of MOR and MET in PBS. The FFT-SWV frequency of 256 Hz and the amplitude of 15 mV.
Figure 9
Figure 9
Results of Calibration and validation by PLS model for (A) MOR and (B) MET.
See this image and copyright information in PMC

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