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HomeThin Layer ChromatographyThin Layer Chromatography Identification Test for Dextromethorphan following European Pharmacopeia Monograph on Silica Gel G 254 Plates

Thin Layer Chromatography Identification Test for Dextromethorphan following European Pharmacopeia Monograph on Silica Gel G 254 Plates

Introduction

Dextromethorphan is a drug of the morphinan class. It is a cough suppressant with sedative, dissociative, and stimulant properties (at higher doses) and it is the active ingredient in many over-the-counter cold and cough medicines.

This application note illustrate how Silica Gel G plates are suitable for the analysis of Dextromethorphan following the European pharmacopeia identification TLC test experimental conditions (version 9.0).

Dextromethorphan Hydrobromide

Figure 1.Dextromethorphan Hydrobromide

TLC PlateSilica Gel 60G F254 20 x 20 cm Injection volume5 µL
DetectionSpray with potassium iodobismuthate solution R2 (Potassium iodobismuthate solution: Suspend 1.7 g of bismuth subnitrate R and 20 g of tartaric acid R in 40 mL of water R. To the suspension add 40 mL of a 400 g/L solution of potassium iodide R and stir for 1 h. Filter. The solution may be kept for several days in brown bottles. Mix immediately before use 5 mL of the stock solution with 15 mL of water.
Mobile PhaseConcentrated ammonia: methanol : methylene chloride : ethyl acetate : toluene 2:13:10:20:55 (v/v/v/v/v )
Development Over 2/3rd of the plate
DiluentMethanol
DryingIn air
StandardDissolve 25 mg of standard timolol maleate in methanol and dilute
to 10 ml with the same solvent
SampleDissolve 25 mg substance to be examined in methanol and dilute
to 10 ml with the same solvent.
Table 1.Experimental Conditions
TLC plate development

Figure 2.TLC plate development

Chromatograms

Figure 3.Chromatograms

Spectrum

Figure 4.Spectrum

Chromatographic Data (Standard Solution)

Figure 5.Chromatographic Data (Standard Solution)

Chromatographic Data (Sample Solution)

Figure 6.Chromatographic Data (Sample Solution)

CompoundRf
1Dextromethorphan0.29
CompoundRf
1Dextromethorphan0.29
STD 12363
STD 22347
STD 32494
STD 42453
STD 52461
Mean2423.6
Standard Deviation64.7
RSD (%)2.7
Table 2.Standard Repeatability
  1. The principal spot in the chromatogram obtained with the test solution is similar in position, colour and size to the principal spot in the chromatogram obtained with reference solution.
  2. All the spots for the reference solution have a repeatability better than 3% RSD.
  3. Merck silica gel G plates provides repeatable and reproducible results for Dextromethorphan identification test and comply to all requirements as per European Pharmacopoeia.

Materials
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