de Oliveira Marcone A L, Solis Victor E S, Gioielli Luiz A, Polakiewicz Bronislaw, Tavares Marina F M
Instituto de Química, Universidade de São Paulo, São Paulo, SP, Brazil.
Electrophoresis. 2003 May;24(10):1641-7. doi: 10.1002/elps.200305394.
A novel capillary electrophoresis methodology using UV indirect detection (224 nm) for the analysis of trans-fatty acids in hydrogenated oils was proposed. The electrolyte consisted of a pH 7 phosphate buffer at 15 mmol x L(-1) concentration containing 4 mmol.L(-1) sodium dodecylbenzenesulfonate, 10 mmol x L(-1) polyoxyethylene 23 lauryl ether (Brij 35), 2% 1-octanol and 45% acetonitrile. Under the optimized conditions, ten fatty acids, C12:0, C13:0 (internal standard), C14:0, C16:0, C18:0, C18:1c, C18:1t, C18:2cc, C18:2tt and C18:3ccc were baseline-separated in less than 12 min. The proposed methodology was applied to monitor the formation of trans-fatty acids during hydrogenation of Brazilnut oil. A crude oil sample (42.1% linoleic acid, 37.3% oleic acid, 13.4% palmitic acid, and 7.0% stearic acid) was mixed with 0.25% of a nickel-based catalyst and submitted to two independent hydrogenation conditions: 175 degrees C, 3 atm, 545 rpm for 60 min (GH(1) sample), and 150 degrees C, 1 atm, 545 rpm for 30 min (GH(2) sample). For the most severe hydrogenation condition (higher temperature and pressure, under longer reactional period), a more complete conversion of linoleic and oleic acids into stearic acid occurred with concomitant formation of the trans-species, elaidic acid (C18:1t). For the milder hydrogenation procedure that generated sample GH(2), larger amounts of linoleic and oleic acids remained, in addition to the transformations already observed in the GH(1) sample.
提出了一种采用紫外间接检测(224nm)的新型毛细管电泳方法,用于分析氢化油中的反式脂肪酸。电解质由浓度为15mmol·L⁻¹的pH 7磷酸盐缓冲液组成,其中含有4mmol·L⁻¹的十二烷基苯磺酸钠、10mmol·L⁻¹的聚氧乙烯23月桂醚(Brij 35)、2%的1-辛醇和45%的乙腈。在优化条件下,十种脂肪酸,即C12:0、C13:0(内标)、C14:0、C16:0、C18:0、C18:1c、C18:1t、C18:2cc、C18:2tt和C18:3ccc在不到12分钟内实现了基线分离。该方法用于监测巴西坚果油氢化过程中反式脂肪酸的形成。将原油样品(42.1%亚油酸、37.3%油酸、13.4%棕榈酸和7.0%硬脂酸)与0.25%的镍基催化剂混合,并进行两种独立的氢化条件:175℃、3个大气压、545转/分钟,反应60分钟(GH(1)样品),以及150℃、1个大气压、545转/分钟,反应30分钟(GH(2)样品)。对于最剧烈的氢化条件(更高的温度和压力,更长的反应时间),亚油酸和油酸更完全地转化为硬脂酸,同时伴随着反式异构体反油酸(C18:1t)的形成。对于生成样品GH(2)的较温和氢化过程,除了在GH(1)样品中已经观察到的转化外,还残留了大量的亚油酸和油酸。