High-performance thin-layer chromatography (HPLTC)–densitometry methods are described for the analysis of the anti(retro)virals dolutegravir (D), lamivudine (L), and tenofovir disoproxil fumarate (TDF) in a pharmaceutical tablet product. To the best of our knowledge, no previous quantitative planar chromatography method has been reported in the literature for this combination formulation. The method for L was transferred from a thin-layer chromatography (TLC) screening method published in the Global Pharma Health Fund (GPHF) Minilab Manual designed for identification of counterfeit and substandard drug products using a model process published earlier. D and TDF are not included in the list of drugs for which TLC screening methods are published for the Minilab, but HPTLC–densitometry procedures were developed for them using the transfer process guidelines. L was analyzed simultaneously with TDF on Merck Premium Purity silica gel 60 F plates using the mobile phase ethyl acetate–methanol–acetone–concentrated ammonium hydroxide (30:7:3:1) and densitometric scanning at 254 nm. D was analyzed on a second plate by scanning at 366 nm after chromatography with the chloroform–methanol–formic acid (32:8:2) mobile phase. Data for all three drugs are shown to meet the requirements of the model transfer process for calibration curve r values, assay of tablets relative to their label values, peak purity/peak identity tests, and validation by standard addition analysis of samples spiked at 50%, 100%, and 150% of the label value of active ingredients. A TLC screening method for TDF in the combination product was developed and published online with open access.
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Transfer of seven thin-layer chromatography (TLC) Global Pharma Health Fund E.V. Minilab protocols for screening counterfeit pharmaceutical products in the field to quantitative high-performance TLC (HPTLC)–densitometry methods was performed using a model process published previously. The developed and validated methods for tablets containing amlodipine besylate, cefpodoxime proxetil, cetirizine 2HCl, diclofenac sodium, efavirenz, mefenamic acid, and atovaquone + proguanil HCl involved the use of only relatively inexpensive and nontoxic solvents, Merck KGaA Premium Purity HPTLC silica gel 60 F254 plates, semi-automated sample and standard solution application with a CAMAG Linomat 4, and automated densitometry with a CAMAG Scanner 3 for detection, identification, and quantification. In addition, previously transferred HPTLC–densitometry methods for azithromycin and for cephalexin were used to analyze a new product of each drug to demonstrate the applicability of the methods.
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