Laakso P, Christie W W
Hannan Research Institute, Ayr. Scotland.
Lipids. 1990 Jun;25(6):349-53. doi: 10.1007/BF02544346.
Diacylglycerols have been separated as their (S)-(+)-or (R)-(-)-1-(1-naphthyl)ethyl urethanes by high performance liquid chromatography (HPLC) on a column of silica gel with 0.5% 2-propanol in hexane as the mobile phase. The elution order of components derivatized with the (S)-form of the reagent was 1,3-, followed by 1,2-, and finally 2,3-diacyl-sn-glycerols. The elution order of 1,2- and 2,3-diasteromers was reversed when the (R)-form of 1-(1-naphthyl)ethyl isocyanate was used for derivatization. Single-acid 1,2- and 2,3-diastereomers were separated to the baseline with a resolution factor from 5.2-5.7, and the resolution factor between 1,3- and 1,2- or 2,3-diacyl-sn-glycerol derivatives was more than 23. Molecular species of single-acid diacylglycerol derivatives were separated in the sequence 18:1 less than 18:0 less than 18:2 less than 16.0. In order to assess this methodology as part of a procedure for the stereospecific analysis of triacyl-sn-glycerols, we prepared diacyl-rac-glycerols from maize oil, evening primrose oil and egg yolk triacylglycerols by partial hydrolysis with ethyl magnesium bromide. The 1,3-, 1,2- and 2,3-diacyl-sn-glycerols as (S)-(+)-1-(1-naphthyl)ethyl urethanes were isolated and their fatty acid compositions were determined. Although this only permitted an indirect determination of the compositions of positions sn-1, -2 and -3, it was sufficient to indicate the potential of the methodology because results comparable to those published earlier were achieved.
通过高效液相色谱(HPLC),以硅胶柱为固定相,0.5%异丙醇的正己烷溶液为流动相,将二酰基甘油分离为它们的(S)-(+)-或(R)-(-)-1-(1-萘基)乙基脲烷。用该试剂的(S)-形式衍生化的组分的洗脱顺序为1,3-二酰基-sn-甘油,接着是1,2-二酰基-sn-甘油,最后是2,3-二酰基-sn-甘油。当使用(R)-1-(1-萘基)乙基异氰酸酯进行衍生化时,1,2-和2,3-非对映异构体的洗脱顺序颠倒。单酸1,2-和2,3-非对映异构体以5.2 - 5.7的分离因子分离至基线,1,3-与1,2-或2,3-二酰基-sn-甘油衍生物之间的分离因子大于23。单酸二酰基甘油衍生物的分子种类按18:1<18:0<18:2<16:0的顺序分离。为了评估该方法作为三酰基-sn-甘油立体特异性分析程序的一部分,我们用乙基溴化镁部分水解玉米油、月见草油和蛋黄三酰基甘油制备了二酰基-rac-甘油。分离出作为(S)-(+)-1-(1-萘基)乙基脲烷的1,3-、1,2-和2,3-二酰基-sn-甘油,并测定了它们的脂肪酸组成。尽管这仅允许间接测定sn-1、-2和-3位的组成,但足以表明该方法的潜力,因为获得了与早期发表的结果相当的数据。