蔬菜中维生素K_1的测定——HPLC法  

DETERMINATION OF VITAMIN K_1 IN VEGETABLES BY HPLC

作　　者：王竹[1] 王光亚[1] 

机构地区：[1]中国预防医学科学院,营养与食品卫生研究所北京100050

出　　处：《营养学报》1999年第4期450-454,共5页Acta Nutrimenta Sinica

基　　金：全国卫生标准委员会资助!No.4-95-217

摘　　要：目的：　为了检测蔬菜中维生素Ｋ１（ＶＫ１）的含量，需建立一个特异性强分离效果好的检测方法。方法：　蔬菜样品经丙酮、石油醚提取后，再用失活磷酸盐处理过的氧化铝进行柱色谱净化处理，分别用极性不同的洗脱液将样品中ＶＫ１ 从干扰物中分离出来，收集石油醚∶乙醚（９７∶３）洗脱组分，浓缩定容。然后用Ｃ１８色谱柱对ＶＫ１ 进行定性定量分析，流动相为甲醇：正己烷（９８∶２），紫外检测波长为２４８ｎｍ 。结果：　在流速为１．５ｍ ｌ／ｍ ｉｎ 的条件下，ＶＫ１ 的保留时间为１５．６ｍ ｉｎ，方法批内、批间ＲＳＤ％ 分别为１．４％ ～６．１％ 和１．３％ ～７．１％ ，回收率范围为９０．９％ ～１０９．３％ 。结论：　采用失活的磷酸盐处理过的氧化铝色谱柱对样品进行净化处理，可以提高分离效果。In order to assay vitamin K 1 in vegetables, a specific determination method with good separation efficiency should be set up. Methods:Vegetable samples were extracted by acetone and petroleum ether, and passed through deactive phosphate treated alumina chromatographic column. Vitamin K 1 in samples was isolated by eluents with different polarity, and then the fraction eluted by petroleum ether: ether (97∶3) was analyzed on a column C 18 of HPLC with UV detector at 248nm. Mobile phase was methanol: hexane (98∶2). Results:Under the flow rate 1.5ml/min, the retention time of VK 1 was 15.6 min. The relative SD RSD% of within run and between run reproducibilities test were 1.4%～6.1%, 1.3%～ 7.1 % respectively, and the recovery rate ranged from 90.9% to 109.3%. Conclusion:The deactive phosphate treated alumina chromatographic column acceptable in purifying samples, which improves extraction efficiency. The method is suitable for analyzing vegetable samples.

关 键 词：蔬菜 维生素K1 高效液相色谱 

分 类 号：R151.3[医药卫生—营养与食品卫生学]