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中国精品科技期刊2020
马蒙蒙, 王宗义, 贾明宏, 王国庆, 盛晔琪, 翟孟婷, 郑宇. 超低温冷冻除脂-气相色谱串联质谱法检测食用植物油中21种邻苯二甲酸酯[J]. 食品工业科技, 2018, 39(12): 271-274,300. DOI: 10.13386/j.issn1002-0306.2018.12.048
引用本文: 马蒙蒙, 王宗义, 贾明宏, 王国庆, 盛晔琪, 翟孟婷, 郑宇. 超低温冷冻除脂-气相色谱串联质谱法检测食用植物油中21种邻苯二甲酸酯[J]. 食品工业科技, 2018, 39(12): 271-274,300. DOI: 10.13386/j.issn1002-0306.2018.12.048
MA Meng-meng, WANG Zong-yi, JIA Ming-hong, WANG Guo-qing, SHENG Ye-qi, ZHAI Meng-ting, ZHENG Yu. Determination of 21 phthalic acid esters in edible vegetable oils by gas chromatography-tandem mass spectrometry with removing fat through ultra low temperature freezing[J]. Science and Technology of Food Industry, 2018, 39(12): 271-274,300. DOI: 10.13386/j.issn1002-0306.2018.12.048
Citation: MA Meng-meng, WANG Zong-yi, JIA Ming-hong, WANG Guo-qing, SHENG Ye-qi, ZHAI Meng-ting, ZHENG Yu. Determination of 21 phthalic acid esters in edible vegetable oils by gas chromatography-tandem mass spectrometry with removing fat through ultra low temperature freezing[J]. Science and Technology of Food Industry, 2018, 39(12): 271-274,300. DOI: 10.13386/j.issn1002-0306.2018.12.048

超低温冷冻除脂-气相色谱串联质谱法检测食用植物油中21种邻苯二甲酸酯

Determination of 21 phthalic acid esters in edible vegetable oils by gas chromatography-tandem mass spectrometry with removing fat through ultra low temperature freezing

  • 摘要: 建立了超低温冷冻除脂-气相色谱串联质谱(GC-MS/MS)检测食用植物油中21种邻苯二甲酸酯(PAEs)的新方法。样品用乙腈提取,经超低温(-80℃)冷冻10 min除脂,再经减压浓缩,以正己烷复溶,采用GC-MS/MS多反应监测模式进行测定。结果表明,在考察浓度范围(1~1000 ng/mL)内21种PAEs均呈现良好线性,相关系数均大于0.999,检出限为0.10~8.52 μg/kg,定量限为0.32~28.40 μg/kg,加标回收率为74.31%~116.62%,相对标准偏差为1.21%~17.82%。对市售7类19个油样的抽样检测,显示邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸(2-丁氧基)乙酯(DBEP)、邻苯二甲酸二正庚酯(DHP)、邻苯二甲酸二(2-乙基己)酯(DEHP)和邻苯二甲酸二正辛酯(DNOP)共9种PAEs被检出,其中DMP、DBP、DBEP、DHP和DEHP检出率均大于90%,含量范围为105.57~2156.76 μg/kg。该方法操作简便,成本低,可用于食用植物油中PAEs的有效测定。

     

    Abstract: A new method was developed for the determination of 21 Phthalic Acid Esters(PAEs)in edible vegetable oils by gas chromatography tandem mass spectrometry(GC-MS/MS)with removing fat through ultra low temperature freezing. With acetonitrile as extractant,sample was extracted and frozen with ultra low temperature at-80℃ for 10 min to remove fat,and then the sample solution was evaporated to near dryness by rotary evaporator and redissolved by n-hexane,and then detected by GC-MS/MS under multiple reaction monitoring modes. All analytes had good linearity with correlation coefficient over 0.999 in the investigated range(1~1000 ng/mL),the limits of detection(LOD)were 0.10~8.52 μg/kg,the limits of quantitation(LOQ)were 0.32~28.40 μg/kg,the recoveries were 74.31%~116.62% with the relative standard deviation ranged of 1.21%~17.82%. Seven categories of 19 kinds of vegetable oil were examined,the results indicated that dimethyl phthalate(DMP),diethyl phthalate(DEP),diisobutylphthalate(DIBP),di-n-butyl phthalate(DBP),butyl benzyl phthalate(BBP),bis(2-butoxyethyl)phthalate(DBEP),di-n-heptyl phthalate(DHP),bis(2-ethylhexyl)phthalate(DEHP)and di-n-octyl phthalate(DNOP)total of 9 PAEs were detected,including DMP,DBP,DBEP,DHP and DEHP detection rate of more than 90% with the content in the range of 105.57~2156.76 μg/kg. The method was easy to operate and low cost,which could be used for the effective determination of PAEs in edible vegetable oil.

     

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