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中国油料作物学报 ›› 2019, Vol. 41 ›› Issue (6): 842-.doi: 10.19802/j.issn.1007-9084.2019177

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Extraction and determination of trans-vitamin K1 in Brassica napus bolt by SPE-HPLC-MS/MS

  

  1. 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
  • Online:2019-12-28 Published:2019-12-20

Abstract:

 To accurately determine the content of trans-vitamin K1, extraction and determination of trans-vita?min K1 in vegetables was developed by using solid phase extraction high performance liquid chromatography-tan?dem mass spectrometry (SPE-HPLC-MS/MS). The target was extracted by n-hexane and purified by neutral alumi?na SPE column, and then separated on aC30 liquid chromatography column with methanol containing 0.025% formic acid and 2.5 mmol/L ammonium formate, and quantified by mass spectrometry in selected reaction monitoring (SRM) mode. The cis- and trans-vitamin K1 were separated within 20 min. The validation results showed that a good relationship in linear ranges was obtained with correlation coefficients of 0.9985. Meanwhile, limit of detection (LOD) and limit of quantification (LOQ) of trans-vitamin K1 were 0.29 μg/kg and 0.95 μg/kg, respectively. The re? covery rates ranged from 87.5% to 117.6%, the relative standard deviations (RSDs) of intra-day and inter-day var? ied from 0.72% to 9.59%. Then, the proposed method was used to analyze bolt of rapeseed (Brassica napus L.)and three other vegetables(B. rapa spp. chinensis, B. oleracea var. Italic Planch, B. oleracea var. capitata)with high content of trans-vitamin K1. The content of trans-vitamin K1 in B. napus was 340.08 μg/100g and higher than those in Chinese cabbage (260.93 μg/100g), broccoli (167.65 μg/100g) and kohlrabi (151.11 μg/100g). The proposed method has high sensitivity and selectivity, and could be successfully employed to detect vitamin K1 in vegetables. The comparison between Brassica napus with other vegetables indicated that Brassica napus is a vegetable with high
vitamin K1 content.

Key words: vitamin K1, Brassica napus bolt, solid phase extraction, liquid chromatography tandem massspectrometry