{"id":678,"date":"2015-02-15T06:35:12","date_gmt":"2015-02-15T06:35:12","guid":{"rendered":"http:\/\/biomedpharmajournal.org\/?p=678"},"modified":"2020-04-25T07:31:26","modified_gmt":"2020-04-25T07:31:26","slug":"electroanalysis-of-nalmefene-and-its-determination-in-pharmaceutical-formulations-and-biological-fluid-samples","status":"publish","type":"post","link":"https:\/\/biomedpharmajournal.org\/staging\/vol2no1\/electroanalysis-of-nalmefene-and-its-determination-in-pharmaceutical-formulations-and-biological-fluid-samples\/","title":{"rendered":"Electroanalysis of Nalmefene and its Determination in Pharmaceutical Formulations and Biological Fluid Samples"},"content":{"rendered":"

Introduction<\/strong><\/p>\n

Nalmefene [17-cyclopropylmethyl-4,5\u03b1-epoxy-6-methylenemorphinan-3,14-diol] \u00a0<\/strong>(NLM) is an opioid antagonist used in the treatment of opioid over dose and postoperative opioid depression.\u00a0 GC-MS (1) and HPLC (2 ) methods were reported for the determination of NLM. But voltammetric\u00a0 methods have not\u00a0 been reported which are simple, rapid and more accurate than the above methods. We reported the determination of drugs based on their electrochemical reduction (3, 4). In the present method, a clay modified carbon paste electrode has been employed because they are able to adsorb and to incorporate electroactive species for the determination of an analyte. (5-10).<\/p>\n

Experimental<\/strong><\/p>\n

Voltammograms were recorded with Metrohm 757 VA computrace (Herisau, Switzerland).Nalmefene (NLM) was purchased from Sigma. Graphite powder (l-2 mm particle size), paraffin oil from Aldrich India Ltd., Bangalore. All chemicals used for the preparation of buffers and supporting electrolytes are of reagent grade.<\/p>\n

Recommended Procedure<\/strong><\/p>\n

An appropriate amount of NLM working standard solution is placed in the electrolytic cell which contained Britton Robinson buffer of pH 3.0. Subsequently a steam of oxygen-free nitrogen gas is passed into the solution for 10 min. The laboratory made working electrode is placed in the cell, during the deposition of the test species the solution is stirred for 150 s at<\/p>\n

-0.4 V. The stirring (2000rpm) is stopped and after 25 s of equilibration time, the cathodic sweep is carried out toward negative potential. All the measurements are made at 21\u00b1 2 \u00b0C.<\/p>\n

Results and Discussion<\/strong><\/p>\n

Cyclic Voltammetry<\/strong><\/p>\n

Fig. 1 \u00a0illustrates the cyclic voltammogram recorded for NLM at carbon paste electrode (CPE) and clay modified carbon paste electrode (CMCPE). On scanning towards a negative potential on a bare carbon paste electrode, only a much smaller cathodic peak is observed. When CMCPE is used a large increase in the peak currents is observed. No peaks are observed in the anodic sweep indicating that the reduction of NLM under investigation is of irreversible.<\/p>\n\n\n\n
\"Figure<\/td>\nFigure 1: Typical CV of\u00a0 NLM at (a) bare CPE; (b) CMCPE.<\/strong><\/p>\n

 <\/p>\n

Click here to View figure<\/a><\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n

 <\/p>\n

Differential Pulse Voltammetry<\/strong><\/p>\n

Fig. 2 \u00a0illustrates differential pulse voltammogram obtained at bare carbon paste electrode and clay modified carbon paste electrodes for NLM in BR buffer of pH 3.0. From the obtained results the peak currents obtained at clay modified carbon paste electrode are almost twice than those at carbon paste electrode of concentration 1.6×10-9<\/sup>M NLM.<\/p>\n\n\n\n
\"Figure<\/td>\nFigure 2:\u00a0Typical DPAdSV of\u00a0NLM (a) \u00a0\u00a0\u00a0bare CPE; (b) CMCPE . <\/strong><\/p>\n

 <\/p>\n

Click here to View figure<\/a><\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n

 <\/p>\n

The peak is attributed \u00a0to the reduction of carbon, carbon double bond according to the currently accepted mechanism for the electroreduction of carbon, carbon double bond containing compounds.(11, 12).<\/p>\n

Scheme.1 Reduction of Nalmefene<\/strong><\/p>\n\n\n\n
\"Scheme<\/td>\nScheme 1: Reduction of Nalmefene.<\/strong><\/p>\n

 <\/p>\n

Click here to View Scheme<\/a><\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n

 <\/p>\n

Effect of pH, Accumulation Potential and Accumulation Time<\/strong><\/p>\n

The results from the overall the experiment show that peak current is maximum at the pH 3.0. The peak currents of NLM increase as the accumulation potential increases from -0.1 V and reaches maximum at -0.4 V; as the Eacc<\/sub> increases further, the ip<\/sub> values started decreasing. Thus, an optimal accumulation potential of-0.4 V is used for further studies.Sharp increasing peak currents are obtained up to accumulation time 300 s and 150 s of NLM at CPE and CMCPE respectively. For longer accumulation times above 300 and 150 s the peak currents practically level off. . So in the further studies, a preconcentration time of 150 s is preferred as effective criteria.<\/p>\n

Table 1: Experimental data of\u00a0 NLM.<\/strong><\/p>\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n
Parameters<\/strong><\/td>\nNLM<\/strong><\/td>\n<\/tr>\n
CPE<\/strong><\/td>\nCMCPE<\/strong><\/td>\n<\/tr>\n
Linearity range (M)<\/strong><\/td>\n2.4 \u00b4 10-8<\/sup> to<\/td>\n1.4 \u00b4 10-9<\/sup> to<\/td>\n<\/tr>\n
1.6 \u00b4 10-5<\/sup><\/td>\n5.2 \u00b4 10-5<\/sup><\/td>\n<\/tr>\n
Calibration curve equation\u00a0<\/strong><\/td>\nY(mA)=0.3035X + 0.0335<\/td>\nY(mA)= 0.9862 X + 0.1195<\/td>\n<\/tr>\n
Correlation coefficient<\/strong><\/td>\n0.9975<\/td>\n0.9982<\/td>\n<\/tr>\n
L.O.D (M)<\/strong><\/td>\n1.6 \u00b4 10-8<\/sup><\/td>\n1.1 \u00b4 10-9<\/sup><\/td>\n<\/tr>\n
L.O.Q (M)<\/strong><\/td>\n0.533 \u00b4 10-7<\/sup><\/td>\n0.334 \u00b4 10-8<\/sup><\/td>\n<\/tr>\n
Repeatability of<\/strong><\/td>\n4.12<\/td>\n4.18<\/td>\n<\/tr>\n
peak currents<\/strong><\/td>\n<\/tr>\n
%RSD)<\/strong><\/td>\n<\/tr>\n
Repeatability of<\/strong><\/td>\n0.43<\/td>\n0.49<\/td>\n<\/tr>\n
Peak potentials<\/strong><\/td>\n<\/tr>\n
%RSD)<\/strong><\/td>\n<\/tr>\n
Reproducibility of peak currents<\/strong><\/td>\n3.51<\/td>\n3.82<\/td>\n<\/tr>\n
%RSD)<\/strong><\/td>\n<\/tr>\n
Reproducibility of potentials<\/strong><\/td>\n0.32<\/td>\n0.41<\/td>\n<\/tr>\n
%RSD)<\/strong><\/td>\n<\/tr>\n
Numbers of assays<\/strong><\/td>\n12<\/td>\n12<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n

 <\/p>\n

Table 2: Chosen Experimental Conditions.<\/strong><\/p>\n\n\n\n\n\n\n\n\n\n\n\n\n\n
Variable<\/strong><\/td>\nChosen Value<\/strong><\/td>\n<\/tr>\n
pH<\/strong><\/td>\n3.0<\/td>\n<\/tr>\n
Buffer volume (ml)<\/strong><\/td>\n10<\/td>\n<\/tr>\n
Temperature (\u00b0C)<\/strong><\/td>\n21<\/td>\n<\/tr>\n
Purge time (s)<\/strong><\/td>\n300<\/td>\n<\/tr>\n
Accumulation potential (V)<\/strong><\/td>\n-0.4<\/td>\n<\/tr>\n
Accumulation time (s)<\/strong><\/td>\n150<\/td>\n<\/tr>\n
Rest time (s)<\/strong><\/td>\n25<\/td>\n<\/tr>\n
Stirring rate (rpm)<\/strong><\/td>\n\u00a0\u00a0 2000<\/td>\n<\/tr>\n
Scan rate (mVs-1<\/sup>)<\/strong><\/td>\n10<\/td>\n<\/tr>\n
Pulse amplitude (mV)<\/strong><\/td>\n50<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n

 <\/p>\n

Table 3: Determination of NLM in Pharmaceutical formulations.<\/strong><\/p>\n\n\n\n\n\n\n
Name of the drug<\/strong><\/td>\nAmount labeled (m.g\/L)<\/strong><\/td>\n*Average amount found<\/strong><\/p>\n

(m.g\/L)<\/strong><\/td>\n

Recovery percentage<\/strong><\/p>\n

(%)<\/strong><\/td>\n

+<\/u> S.D<\/strong><\/td>\nRSD<\/strong><\/td>\n<\/tr>\n
NLM<\/td>\n2<\/td>\n1.956<\/td>\n97.8<\/td>\n0.0152<\/td>\n0.78<\/td>\n<\/tr>\n
<\/td>\n4<\/td>\n3.923<\/td>\n98.07<\/td>\n0.0602<\/td>\n1.534<\/td>\n<\/tr>\n
<\/td>\n6<\/td>\n5.80<\/td>\n96.66<\/td>\n0.0670<\/td>\n1.155<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n

 <\/p>\n

Table 4 : Determination of NLM in spiked human serum samples.<\/strong><\/p>\n\n\n\n\n\n\n
Name of the drug<\/strong><\/td>\nAmount Spiked (m.g\/L)<\/strong><\/td>\n*Average amount found<\/strong><\/p>\n

(m.g\/L)<\/strong><\/td>\n

Recovery percentage<\/strong><\/p>\n

(%)<\/strong><\/td>\n

+<\/u> S.D<\/strong><\/td>\nRSD<\/strong><\/td>\n<\/tr>\n
NLM<\/td>\n2<\/td>\n1.987<\/td>\n99.35<\/td>\n0.0152<\/td>\n0.765<\/td>\n<\/tr>\n
<\/td>\n6<\/td>\n5.957<\/td>\n99.28<\/td>\n0.0251<\/td>\n0.4213<\/td>\n<\/tr>\n
<\/td>\n10<\/td>\n9.933<\/td>\n99.33<\/td>\n0.0321<\/td>\n0.323<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n

 <\/p>\n

Table 5: Determination of NLM in spiked human serum samples<\/strong><\/p>\n\n\n\n\n\n\n
Name of the drug<\/strong><\/td>\nAmount Spiked (m.g\/L)<\/strong><\/td>\n*Average amount found<\/strong><\/p>\n

(m.g\/L)<\/strong><\/td>\n

Recovery percentage<\/strong><\/p>\n

(%)<\/strong><\/td>\n

+<\/u> S.D<\/strong><\/td>\nRSD<\/strong><\/td>\n<\/tr>\n
NLM<\/td>\n2<\/td>\n1.981<\/td>\n99.05<\/td>\n0.022<\/td>\n1.1<\/td>\n<\/tr>\n
<\/td>\n4<\/td>\n3.90<\/td>\n97.50<\/td>\n0.0353<\/td>\n0.905<\/td>\n<\/tr>\n
<\/td>\n6<\/td>\n3.892<\/td>\n97.3<\/td>\n0.033<\/td>\n0.84<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n

\u00a0<\/strong><\/p>\n

Conclusion<\/strong><\/p>\n

Higher sensitivity has achieved at CMCPE when compared to CPE. The irreversibility of reduction behavior of NLM has been investigated. The present method has been compared with already existing methods for the determination of NLM\u00a0 and found better recovery, more accurate, more sensitive and achieved at lower detection limits.<\/p>\n

References<\/strong><\/p>\n

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    Introduction Nalmefene [17-cyclopropylmethyl-4,5\u03b1-epoxy-6-methylenemorphinan-3,14-diol] \u00a0(NLM) is an opioid antagonist used in […]<\/p>\n","protected":false},"author":2,"featured_media":0,"comment_status":"closed","ping_status":"closed","sticky":false,"template":"","format":"standard","meta":{"footnotes":""},"categories":[6],"tags":[],"class_list":["post-678","post","type-post","status-publish","format-standard","hentry","category-vol2no1"],"_links":{"self":[{"href":"https:\/\/biomedpharmajournal.org\/staging\/wp-json\/wp\/v2\/posts\/678","targetHints":{"allow":["GET"]}}],"collection":[{"href":"https:\/\/biomedpharmajournal.org\/staging\/wp-json\/wp\/v2\/posts"}],"about":[{"href":"https:\/\/biomedpharmajournal.org\/staging\/wp-json\/wp\/v2\/types\/post"}],"author":[{"embeddable":true,"href":"https:\/\/biomedpharmajournal.org\/staging\/wp-json\/wp\/v2\/users\/2"}],"replies":[{"embeddable":true,"href":"https:\/\/biomedpharmajournal.org\/staging\/wp-json\/wp\/v2\/comments?post=678"}],"version-history":[{"count":5,"href":"https:\/\/biomedpharmajournal.org\/staging\/wp-json\/wp\/v2\/posts\/678\/revisions"}],"predecessor-version":[{"id":32987,"href":"https:\/\/biomedpharmajournal.org\/staging\/wp-json\/wp\/v2\/posts\/678\/revisions\/32987"}],"wp:attachment":[{"href":"https:\/\/biomedpharmajournal.org\/staging\/wp-json\/wp\/v2\/media?parent=678"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/biomedpharmajournal.org\/staging\/wp-json\/wp\/v2\/categories?post=678"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/biomedpharmajournal.org\/staging\/wp-json\/wp\/v2\/tags?post=678"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}