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Aluda AT, Amugune BK, Abuga KO, Kamau FN. "Development and Validation of a Gas Chromatographic Method for Determination of Menthol in Cold-Cough Syrups." PJK. 2018;23(3):90-93. Abstract

Background
Common cold is the most common infection of the upper respiratory tract and cold-cough syrups are often prescribed. Although menthol is one of the common constituents of these syrups, quality checks on cold-cough syrups normally target the major active pharmaceutical ingredients without regard to menthol content.

Objective
To develop and validate a gas chromatography method for determination of menthol in cold-cough syrups.

Methods
A simple, rapid, robust, accurate and reliable Gas Chromatography method was developed and validated for the determination of menthol in cold-cough syrups that may also contain ambroxol, chlorpheniramine, guaifenesin, bromhexine and salbutamol.

Results
Optimized chromatographic conditions were: A ZB-WAXplus 60m ×0.25mm; 0.25μm fused silica capillary column. Oven temperature program of 110 0C (2 min), ramp 10 0C/min to 190 0C (2 min). Injector port temperature maintained at 240 0C. Injection volume of 1.0 μl split in the ratio of 50:1. Carrier gas as nitrogen at 1.0mL/min which also serves as make up gas (30 mL/min) in the flame ionization detector (260 0C). Other detector gases were hydrogen (30 mL/ min) and industrial air (300 mL/ min) and the diluent for samples and standards was grade chloroform.
From recovery studies, 97.56 to 102.97 % recovery was reported. Repeatability studies had a coefficient of variation of 0.55 while intermediate precision was 0.32. The method was linear over a range of 0.042 to 0.169 mg/mL with a coefficient of determination (R2) 0.9986.
Of the 21 samples analyzed, only 10 samples (47.6 %) complied with assay specifications of 90.0 to 110.0 % label claim for finished products according to the United States Pharmacopeia 2016.

Conclusion and recommendation
A gas chromatographic method was developed and validated for the determination of menthol in cold-cough syrups in Kenya. This method can be used together with a validated high-performance liquid chromatography method to assay cold-cough syrups that may also contain ambroxol, bromhexine, chlorpheniramine maleate, guaifenesin and salbutamol.
This method can be useful in routine analysis such as pre-registration studies as well as post market surveillance to curb substandard and counterfeit cold-cough syrups.

Kuballa T, Hausler T, Okaru AO, Neufeld M, Abuga KO, Kibwage IO, Rehm J, Luy B, Walch SG, Lachenmeier DW. "Detection of counterfeit brand spirits using 1H NMR fingerprints in comparison to sensory analysis." Food Chem.. 2018;245:112-115. Abstract

Beverage fraud involving counterfeiting of brand spirits is an increasing problem not only due to deception of the consumer but also because it poses health risks e.g. from possible methanol admixture. Suspicious spirit samples from Russia and Kenya were analysed using 1H nuclear magnetic resonance (NMR) spectroscopy in comparison to authentic products. Using linear regression analysis of spectral integral values, 4 counterfeited samples from Russia and 2 from Kenya were easily identifiable with R2 < 0.7. Sensory analysis using triangle test methodology confirmed significant taste differences between counterfeited and authentic samples but the assessors were unable to correctly identify the counterfeited product in the majority of cases. An important conclusion is that consumers cannot assumed to be self-responsible when consuming counterfeit alcohol because there is no general ability to organoleptically detect counterfeit alcohol. Beverage fraud involving counterfeiting of brand spirits is an increasing problem not only due to deception of the consumer but also because it poses health risks e.g. from possible methanol admixture. Suspicious spirit samples from Russia and Kenya were analysed using 1H nuclear magnetic resonance (NMR) spectroscopy in comparison to authentic products. Using linear regression analysis of spectral integral values, 4 counterfeited samples from Russia and 2 from Kenya were easily identifiable with R2 < 0.7. Sensory analysis using triangle test methodology confirmed significant taste differences between counterfeited and authentic samples but the assessors were unable to correctly identify the counterfeited product in the majority of cases. An important conclusion is that consumers cannot assumed to be self-responsible when consuming counterfeit alcohol because there is no general ability to organoleptically detect counterfeit alcohol.

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