In the last years commerce of herbal products as integrators or substitutes for drugs has grown up greatly. The need of active principle quality control methods is so become imperative. The aim of our work was to develop a screening method on the basis of some cases of identification of undeclared drug molecules present in herbal preparations, with important toxicological implications. The first case of examined products dealt about herbal preparations for erection disorders. A number of compounds belonging to phosphodiesterase inhibitors were identified and quantified. Significantly, many of these structures are not factual drugs but unregistered analogues, in some cases coming from illicit commerce: On that occasion traditional analytical methods failed in structural recognition. Multiple stage mass spectrometry shows on the contrary irreplaceable features in rapid drug class identification. For example in MS3 fragmentation of hydroxyhomosildenafil, analogue of the best-known sildenafil, are generated ions typical of MS2 fragmentation pathway of the latter. Another case refers to the undeclared presence of synthetic quaternary disinfectant compounds in various grapefruit-based preparations. A simple LC/ESI-MS/MS multiresidue method has been developed to detect grapefruit bio-markers and a number of quaternary drug molecules in a single analytical run. The application of the herein developed gradient LC-MS/MS method to different herbal products (dry extracts, tablets, emulsions), after dilution or simple liquid extraction, allowed identifying a lot of counterfeit drug preparations, both with commercially known and unknown active substances. In other cases, the presence of plant markers and/or active principles was efficiently confirmed.
Counterfeit drugs identification in herbal products by HPLC-MSn
GIANCOTTI, Valeria Rachele;MASSOLINO, CRISTINA;BAIOCCHI, Claudio;MEDANA, Claudio
2006-01-01
Abstract
In the last years commerce of herbal products as integrators or substitutes for drugs has grown up greatly. The need of active principle quality control methods is so become imperative. The aim of our work was to develop a screening method on the basis of some cases of identification of undeclared drug molecules present in herbal preparations, with important toxicological implications. The first case of examined products dealt about herbal preparations for erection disorders. A number of compounds belonging to phosphodiesterase inhibitors were identified and quantified. Significantly, many of these structures are not factual drugs but unregistered analogues, in some cases coming from illicit commerce: On that occasion traditional analytical methods failed in structural recognition. Multiple stage mass spectrometry shows on the contrary irreplaceable features in rapid drug class identification. For example in MS3 fragmentation of hydroxyhomosildenafil, analogue of the best-known sildenafil, are generated ions typical of MS2 fragmentation pathway of the latter. Another case refers to the undeclared presence of synthetic quaternary disinfectant compounds in various grapefruit-based preparations. A simple LC/ESI-MS/MS multiresidue method has been developed to detect grapefruit bio-markers and a number of quaternary drug molecules in a single analytical run. The application of the herein developed gradient LC-MS/MS method to different herbal products (dry extracts, tablets, emulsions), after dilution or simple liquid extraction, allowed identifying a lot of counterfeit drug preparations, both with commercially known and unknown active substances. In other cases, the presence of plant markers and/or active principles was efficiently confirmed.
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