| 周红茹,孙雪梅,周克茹，等.C18色谱柱去除3-氯-1,2-丙二醇酯测定中的干扰组分[J].中国油脂,2014,39(6):.[ZHOU Hongru,SUN Xuemei,ZHOU Keru，etc.Removal of interfering components by C18 column in determination of 3-chloropropane-1,2-diol fatty acid esters[J].China Oils and Fats,2014,39(6):.] |
| C18色谱柱去除3-氯-1,2-丙二醇酯测定中的干扰组分 |
| Removal of interfering components by C18 column in determination of 3-chloropropane-1,2-diol fatty acid esters |
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| DOI： |
| 中文关键词: 3-氯-1,2-丙二醇酯 C18色谱柱 干扰组分 HPLC |
| 英文关键词:3-chloropropane-1,2-diol fatty acid esters C18 column interfering component HPLC |
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| 中文摘要: |
| 为了在油脂3-氯-1,2-丙二醇酯含量测定中通过预分离过程去除干扰组分，研究对比了固相萃取柱与硅胶柱层析对油样的分离效果。结果表明：油样的乙腈提取液用SunFireTM?C18?色谱柱（4.6?mm×150?mm,?5?μm）分离，以乙腈-异丙醇（体积比1∶1）为流动相，等度洗脱，柱温30℃，流速1?mL/min的HPLC条件下，可以将不同极性的组分进行分离，从而有效去除3-氯-1,2-丙二醇酯测定中的干扰组分。在自制油样中分别添加800、1?000?mg/kg和?1?200?mg/kg的3-氯-1,2-丙二醇酯标准品进行加标回收试验，1,2-二油酸酰-3-氯丙二醇的加标回收率在86.4%～113.7%，1-硬脂酰-3-氯丙二醇的加标回收率在88.4%～105.6%，相对标准偏差均在15%以内。该法耗用溶剂量少且周期较短，可用于大量样本3-氯-1,2-丙二醇酯测定中干扰组分的去除。 |
| 英文摘要: |
| The?effects?of?solid?phase?extraction?column?and?sillca?gel?column?chromatography?on?the?separation?of?oil?sample?were?studied?and?compared?so?as?to?remove?the?interfering?components?from?oil?by?preseparation?process?in?the?determination?of?3-chloropropane-1,2-diol?fatty?acid?esters?(3-MCPDE).?The?results?showed?that?the?acetonitrile?extract?of?oil?sample?was?separated?by?SunFireTM?C18?column?(4.6?mm×150?mm,?5?μm),?then?different?polar?components?in?oil?sample?could?be?separated?under?the?HPLC?conditions?of?mobile?phase?acetonitrile-isopropanol(volume?ratio?1∶1)，?isocratic?elution,?column?temperature?30℃?and?flow?rate?1?mL/min,?thereby?the?interfering?components?were?removed?effectively?in?the?determination?of?3-MCPDE.?The?recovery?experiments?were?conducted?by?adding?800,?1?000?mg/kg?and?1?200?mg/kg?of?3-MCPDE?standards?to?self-made?oil?sample?respectively,?the?recovery?rates?of?1,2-dioleoyl-3-chloropropanediol?and?1-stearoyl-3-chloropropanediol?were?86.4%-113.7%?and?88.4%-105.6%?respectively,and?the?relative?standard?deviations?were?less?than?15%.Therefore,?it?was?feasible?for?removing?the?interfering?components?from?oil?samples?in?determination?of?3-MCPDE?by?C18?column?and?solid?phase?extraction?method?with ?few?solvent?consumption?and?short?processing?cycle. |
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