C18色谱柱去除3-氯-1,2-丙二醇酯测定中的干扰组分

摘要

The effects of solid phase extraction column and sillca gel column chromatography on the sepa-ration of oil sample were studied and compared so as to remove the interfering components from oil by pre-separation 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, 5μm), 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.%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，5μm)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、1000 mg/kg和1200 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。