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
  
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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Author NameAffiliation
ZHOU Hongru  
SUN Xuemei  
ZHOU Keru,etc  
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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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