中国油脂
中國油脂
중국유지
CHINA OILS AND FATS
2014年
6期
85-91
,共7页
周红茹%孙雪梅%周克茹%金青哲%王兴国%徐学兵
週紅茹%孫雪梅%週剋茹%金青哲%王興國%徐學兵
주홍여%손설매%주극여%금청철%왕흥국%서학병
3-氯-1 ,2-丙二醇酯%C18色谱柱%干扰组分%HPLC
3-氯-1 ,2-丙二醇酯%C18色譜柱%榦擾組分%HPLC
3-록-1 ,2-병이순지%C18색보주%간우조분%HPLC
3 - chloropropane -1,2 - diol fatty acid esters%C18 column%interfering component%HPLC
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。
為瞭在油脂3-氯-1,2-丙二醇酯含量測定中通過預分離過程去除榦擾組分,研究對比瞭固相萃取柱與硅膠柱層析對油樣的分離效果。結果錶明:油樣的乙腈提取液用SunFireTM C18色譜柱(4.6 mm ×150 mm,5μm)分離,以乙腈-異丙醇(體積比1:1)為流動相,等度洗脫,柱溫30℃,流速1 mL/min的HPLC條件下,可以將不同極性的組分進行分離,從而有效去除3-氯-1,2-丙二醇酯測定中的榦擾組分。在自製油樣中分彆添加800、1000 mg/kg和1200 mg/kg的3-氯-1,2-丙二醇酯標準品進行加標迴收試驗,1,2-二油痠酰-3-氯丙二醇的加標迴收率在86.4%~113.7%,1-硬脂酰-3-氯丙二醇的加標迴收率在88.4%~105.6%,相對標準偏差均在15%以內。該法耗用溶劑量少且週期較短,可用于大量樣本3-氯-1,2-丙二醇酯測定中榦擾組分的去除。
위료재유지3-록-1,2-병이순지함량측정중통과예분리과정거제간우조분,연구대비료고상췌취주여규효주층석대유양적분리효과。결과표명:유양적을정제취액용SunFireTM C18색보주(4.6 mm ×150 mm,5μm)분리,이을정-이병순(체적비1:1)위류동상,등도세탈,주온30℃,류속1 mL/min적HPLC조건하,가이장불동겁성적조분진행분리,종이유효거제3-록-1,2-병이순지측정중적간우조분。재자제유양중분별첨가800、1000 mg/kg화1200 mg/kg적3-록-1,2-병이순지표준품진행가표회수시험,1,2-이유산선-3-록병이순적가표회수솔재86.4%~113.7%,1-경지선-3-록병이순적가표회수솔재88.4%~105.6%,상대표준편차균재15%이내。해법모용용제량소차주기교단,가용우대량양본3-록-1,2-병이순지측정중간우조분적거제。
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.