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Assessment, Validation and Application to Real Samples of an RP-HPLC Method for the Determination of Guayulins A, B, C and D in Guayule Shrub

Dipartimento di Chimica e Farmacia, Università degli Studi di Sassari, via Vienna 2, 07100 Sassari, Italy
Dipartimento di Scienze Chimiche e Geologiche, Cittadella Universitaria di Monserrato, 09042 Monserrato, Italy
Instituto de Investigaciones en Materiales UNAM, Circuito Exterior Ciudad Universitaria, CP 04510 Mexico DF, Mexico
Facultad de Ciencias Biológicas, Universidad Juárez del Estado de Durango, 35010 Gómez Palacio, Mexico
Authors to whom correspondence should be addressed.
Separations 2018, 5(2), 23;
Received: 25 February 2018 / Revised: 20 March 2018 / Accepted: 22 March 2018 / Published: 9 April 2018
(This article belongs to the Special Issue Chromatographic Techniques for Food and Environmental Samples)
Guayule (Parthenium argentatum Gray) is a shrub native to the arid regions of Mexico. In the last decades, significant attention to its cultivation has arisen because it is the raw material for the production of hypoallergenic natural rubber. Guayule biomass also contains high amounts of resin, which is not normally exploited in any way. Among other sesquiterpenic esters, guayulins (i.e., the parteniol esters of cinnamic acid, guayulin A, or of anisic acid, guayulin B) are contained in resin. In addition, minor amounts of guayulin C and guayulin D are formed by degradation/oxidation of guayulins A and B, respectively. Guayulins likely act as cinnamate and p-anisate reservoirs for the Guayule shrub; in addition, it has been postulated that they might have a key role in the chemical defense system of Guayule. Furthermore, it seems reasonable that guayulins may possess significant biological properties (e.g., antibacterial and anticancer activities), in close analogy with those shown by sesquiterpene lactones contained in many other species of Parthenum genus. As a matter of fact, guayulins A and B play an important role in the synthesis of antineoplastics used in breast cancer treatment. In this contribution we propose an original and validated RP-HPLC approach to the simultaneous quantification of guayulins A, B, C and D. The procedure of resin extraction from Guayule biomass has been optimized in terms of both extraction method and solvent. RP-HPLC separation has been accomplished by an Ascentis® C18 column under isocratic elution with a 80:20 (v:v) acetonitrile:water mixture. Validation was carried out in terms of limits of detection and quantification, linearity, precision, and trueness. Finally, the method was tested with a number of fresh and seasoned samples of spontaneous Guayule shrub from Mexico. View Full-Text
Keywords: guayule; Parthenium argentatum Gray; resin; guayulins; RP-HPLC guayule; Parthenium argentatum Gray; resin; guayulins; RP-HPLC
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Spano, N.; Meloni, P.; Idda, I.; Mariani, A.; Pilo, M.I.; Nurchi, V.M.; Lachowicz, J.I.; Rivera, E.; Orona-Espino, A.; Sanna, G. Assessment, Validation and Application to Real Samples of an RP-HPLC Method for the Determination of Guayulins A, B, C and D in Guayule Shrub. Separations 2018, 5, 23.

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