Development of New HS–SPME–GC–MS Technique to the Measurement of Volatile Terpenoid Profile of Milk

Abstract

This study presented the development of such a HS–SPME–GC–MS technique, with the use of which, directly from the raw milk sample matrix, both qualitatively and quantitatively; the volatile terpenoids (α-pinene, sabinene, β-pinene, p-cymene, limonene, linalool, α-thujene, camphor, menthol, methyl chavicol, caryophyllene E, α-humulene) can be determined, derived from herbs eaten by the dairy animals by different feeding methods. Repeatability was less than 10% in the case of milk fat samples. The estimated limits of quantitation were between 2 and 16 ng/g. The lowest values were 2 ng/g for p-cymene and methyl chavicol; the highest value was 16 ng/g for caryophyllene. In the case of goat milk, the repeatability was better than 8% except for α-thujene. The estimated limits of quantitation were between 1 and 8 ng/g. The lowest values were 1 ng/g for β-pinene, p-cymene and limonene, and the highest value was 8 ng/g for linalool. In milk fat, the highest concentration was identified in caryophyllene E (470 ng/g) and α-humulene (430 ng/g), while the lowest concentration was in p-cymene (2 ng/g) and camphor (2 ng/g). In goat milk, limonene was present in all samples, but its amount varied depending on the type of consumed herb. Methyl chavicol and caryophyllene E were detected in goat’s milk only in one case. The former was detected in sage milk at 2.09 ng/g and the latter in tarragon milk at 2.28 ng/g. We have also successfully demonstrated that the feed consumed by dairy animals also affects the quality of dairy products.