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Abstract: Bovine milk is considered to be a good dietary source of vitamins A, E and β-carotene. This paper describes a robust method for the simultaneous determination of these compounds using high performance liquid chromatography–ion trap mass spectrometry (HPLC–MS n ) as the determinative step. The compounds were separated with a 5μm Polaris 2.1×150mm C18-A column and an aqueous-methanol mobile phase and the levels determined using the MS2 fragments (vitamin A, m/z 213 and m/z 199, vitamin E m/z 165 and β-carotene m/z 413). The HPLC–MS n was operated in the positive ion APCI mode. The method was validated using repeatability studies, duplicate analyses, recovery experiments, proficiency study data and comparison with previously validated high performance liquid chromatographic ultraviolet/visible (HPLC–UV/Vis) and fluorescence (HPLC–Fl) procedures used in our laboratory. Expanded measurement uncertainties were similar for HPLC–MS n , HPLC–UV/Vis and HPLC–Fl, e.g. vitamin A 45μg/100ml, HPLC–MS n ±8%, HPLC–UV ±9%; vitamin E 150μg/100ml, HPLC–MS n ±11%, HPLC–Fl ±9%; β-carotene 12μg/100ml, HPLC–MS n ±18%, HPLC–Vis ±21%. [Copyright &y& Elsevier]

Abstract: A renewed international interest in vitamin D status has revealed significant deficiencies in several populations, including Australia. Vitamin D exists in two forms, cholcalciferol (D3) and ergocalciferol (D2). The main source of vitamin D3 is from exposure of 7-dehydrocholesterol present in the skin to UV irradiation. However, there is an absolute requirement for vitamin D through proper dietary intake if humans live in the absence of sunlight or exclusively indoors. Bovine milk is considered to be a good dietary source of vitamin D3, even though the levels are quite low. This paper describes robust methods using liquid chromatography–linear ion trap mass spectrometry (LC–MSn) and liquid chromatography–tandem mass spectrometry (LC–MS/MS) to measure the levels of vitamin D3 in fresh bovine milk (0.05μg/100ml), commercial (natural and fortified) milk samples (0.01–2μg/100ml) and a dairy based infant formula (8μg/100g), without the need for extensive clean-up procedures. The limits of quantification (LOQ) are 0.01μg/100ml and 0.02μg/100ml for LC–MSn and LC–MS/MS, respectively. Recoveries of vitamin D3 added to the samples prior to saponification were satisfactory (range 60–90%). 25-Hydroxyvitamin D3 was not present in any of the samples analysed (LOQ=0.01μg/100ml, recovery range 30–40%). [ABSTRACT FROM AUTHOR]