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Health-related nutritional human studies rely on the validity of dietary data provided by study participants. Reliable biomarkers for food intake help objectify data collected by food frequency questionnaires. They facilitate the monitoring of compliance with the study requirements, e.g., abstinence from food, help clean biased data, and remove non-compliant individuals. Biomarker candidates are often revealed by sophisticated metabolomics analyses of body fluids, e.g., urine or plasma, collected from case and control study populations. However, validation for using a biomarker candidate in real-life scenarios is seldomly executed. Coffee is a food item of high interest because of the abundance of bioactive compounds and the regularity of life-time consumption by a large part of the population. Coffee has been found to positively impact cardiovascular risk, type 2 diabetes, and cognitive decline. Coffee and its health implications, therefore, are of high interest. A suitable dietary biomarker for coffee consumption is desirable for the clear classification of study participants as coffee drinkers or non-coffee drinkers to enable correlation of physiological response to dietary habits, e.g., coffee consumption. Here, we propose the roast coffee compound N-methylpyridinium (NMP) as a promising biomarker of pragmatic use to distinguish a coffee drinker from a non-coffee drinker. NMP is an easily accessible analytical target from the plasma and urine matrix that can help determine precedent exposure to roasted coffee products. We review the published information on the coffee compound N-methylpyridinium in foods, coffee, and plasma/urine after coffee consumption, and evaluate the data in the context of the proposed food biomarker criteria "plausibility", "time- and dose–response", "robustness", "reliability", "stability", "analytical performance", and "reproducibility". An additional data set is acquired to fill the gaps in the literature. In summary, we conclude that the abundance of NMP can serve as a reliable analytical tool to verify recent consumption of roasted coffee. The use of NMP appears limited to being qualitative, as NMP abundance in coffee and human biosamples is affected by several parameters, e.g., the roasting conditions and the volume and time of coffee consumed. [ABSTRACT FROM AUTHOR]

Health-related nutritional human studies rely on the validity of dietary data provided by study participants. Reliable biomarkers for food intake help objectify data collected by food frequency questionnaires. They facilitate the monitoring of compliance with the study requirements, e.g., abstinence from food, help clean biased data, and remove non-compliant individuals. Biomarker candidates are often revealed by sophisticated metabolomics analyses of body fluids, e.g., urine or plasma, collected from case and control study populations. However, validation for using a biomarker candidate in real-life scenarios is seldomly executed. Coffee is a food item of high interest because of the abundance of bioactive compounds and the regularity of life-time consumption by a large part of the population. Coffee has been found to positively impact cardiovascular risk, type 2 diabetes, and cognitive decline. Coffee and its health implications, therefore, are of high interest. A suitable dietary biomarker for coffee consumption is desirable for the clear classification of study participants as coffee drinkers or non-coffee drinkers to enable correlation of physiological response to dietary habits, e.g., coffee consumption. Here, we propose the roast coffee compound N-methylpyridinium (NMP) as a promising biomarker of pragmatic use to distinguish a coffee drinker from a non-coffee drinker. NMP is an easily accessible analytical target from the plasma and urine matrix that can help determine precedent exposure to roasted coffee products. We review the published information on the coffee compound N-methylpyridinium in foods, coffee, and plasma/urine after coffee consumption, and evaluate the data in the context of the proposed food biomarker criteria “plausibility”, “time- and dose–response”, “robustness”, “reliability”, “stability”, “analytical performance”, and “reproducibility”. An additional data set is acquired to fill the gaps in the literature. In summary, we conclude that the abundance of NMP can serve as a reliable analytical tool to verify recent consumption of roasted coffee. The use of NMP appears limited to being qualitative, as NMP abundance in coffee and human biosamples is affected by several parameters, e.g., the roasting conditions and the volume and time of coffee consumed.

The coffee phytochemical trigonelline and its roasting products nicotinic acid and N -methylpyridinium represent an important class of bioactives that mediate the health benefits of coffee consumption. However, there is a paucity of methods for their simultaneous analysis in coffee beans, especially those affordable and reliable for widespread routine use. To improve this situation, an easy-to-use HPLC−UV method was developed in this study based on a reversed-phase/cation-exchange mixed-mode column showing unique chromatographic selectivity toward the polar and ionic analytes over the matrix components of coffee. The selectivity was achieved by using a decreasing acetonitrile gradient, which tuned the column to a cation-exchange/hydrophilic interaction (CEX/HILIC) mixed separation mode whilst minimizing its hydrophobic interaction capability. The method was assessed for figures of merit, giving limits of detection in coffee beans at around the 0.1 mg/100 g wet matter level, and verified for its applicability to a heterogeneous set of coffee bean samples differing in roasting degree and origin. [Display omitted] • Retention mechanism on the column is selectable between CEX/HILIC and CEX/RP. • CEX/HILIC mixed mode offers selectivity for polar ionic analytes over coffee matrix. • The method proved its applicability to green and roasted coffee with low LOD. • Strong negative correlation existed between trigonelline and the two roast products. [ABSTRACT FROM AUTHOR]