Next Article in Journal
P-TEFb as A Promising Therapeutic Target
Previous Article in Journal
Comparative Assessment of Phytochemical Profiles of Comfrey (Symphytum officinale L.) Root Extracts Obtained by Different Extraction Techniques
Previous Article in Special Issue
Phenolic Profile, Antioxidant and Anti-Proliferative Activities of Methanolic Extracts from Asclepias linaria Cav. Leaves
Open AccessArticle

Extraction and Determination of Vitamin K1 in Foods by Ultrasound-Assisted Extraction, SPE, and LC-MS/MS

by Yueqing Xu 1,2, Liangxiao Zhang 1,3,4,*, Ruinan Yang 1,2, Xu Yu 1,2, Li Yu 1,4, Fei Ma 1,3, Hui Li 1,5, Xiupin Wang 1,4 and Peiwu Li 1,3,4,5
1
Oil Crops Research Institute, Chinese Academy of Agricultural Sciences, Wuhan 430062, China
2
Key Laboratory of Biology and Genetic Improvement of Oil Crops, Ministry of Agriculture and Rural Affairs, Wuhan 430062, China
3
Laboratory of Quality and Safety Risk Assessment for Oilseed Products (Wuhan), Ministry of Agriculture and Rural Affairs, Wuhan 430062, China
4
Quality Inspection and Test Center for Oilseed Products, Ministry of Agriculture and Rural Affairs, Wuhan 430062, China
5
Key Laboratory of Detection for Mycotoxins, Ministry of Agriculture and Rural Affairs, Wuhan 430062, China
*
Author to whom correspondence should be addressed.
Academic Editors: Monika Waksmundzka-Hajnos and Miroslaw Hawryl
Molecules 2020, 25(4), 839; https://doi.org/10.3390/molecules25040839 (registering DOI)
Received: 29 December 2019 / Revised: 11 February 2020 / Accepted: 11 February 2020 / Published: 14 February 2020
(This article belongs to the Special Issue Chromatographic Science of Natural Products)
Vitamin K1 is one of the important hydrophobic vitamins in fat-containing foods. Traditionally, lipase is employed in the determination of vitamin K1 to remove the lipids, which makes the detection complex, time-consuming, and insensitive. In this study, the determination of vitamin K1 in fat-containing foods was developed based on ultrasound-assisted extraction (UAE), solid-phase extraction (SPE) combined with liquid chromatography–tandem mass spectrometry (LC-MS/MS). The optimal conditions for extraction of vitamin K1 were material–liquid ratio of 1:70 (g/mL), extraction temperature of 50 °C, extraction power of 700 W, extraction time of 50 min, material-wash fluid ratio of 1:60 (g/mL), and 8 mL of hexane/anhydrous ether (97:3, v/v) as the elution solvent. Then, vitamin K1 was analyzed on a ZORBAX SB-C18 column (50 mm × 2.1 mm, 1.8 μm) by gradient elution with water (0.01% formic acid) and methanol (0.01 formic acid + 2.5 mmol/L ammonium formate) as the mobile phase. The limit of detection (LOD) and limit of quantification (LOQ) were 0.05 and 0.16 μg/kg, respectively. Calibration curve was linear over the range of 10–500 ng/mL (R2 > 0.9988). The recoveries at three spiked levels were between 80.9% and 119.1%. The validation and application indicated that the proposed method was simple and sensitive in determination of vitamin K1 in fat-containing foods. View Full-Text
Keywords: ultrasound-assisted extraction; solid-phase extraction; LC-MS/MS; vitamin K1; foods ultrasound-assisted extraction; solid-phase extraction; LC-MS/MS; vitamin K1; foods
Show Figures

Figure 1

MDPI and ACS Style

Xu, Y.; Zhang, L.; Yang, R.; Yu, X.; Yu, L.; Ma, F.; Li, H.; Wang, X.; Li, P. Extraction and Determination of Vitamin K1 in Foods by Ultrasound-Assisted Extraction, SPE, and LC-MS/MS. Molecules 2020, 25, 839.

Show more citation formats Show less citations formats
Note that from the first issue of 2016, MDPI journals use article numbers instead of page numbers. See further details here.

Article Access Map by Country/Region

1
Back to TopTop