食品科学

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固相萃取-高效液相色谱法检测油炸猪肉中丙烯酰胺

邵美丽1,郝星宇1,刘 巍1,2,崔承远1,袁兆丰1,董 鑫1   

  1. 1.东北农业大学食品学院,哈尔滨 黑龙江 150030;2.佳木斯出入境检验检疫局,黑龙江 佳木斯 154002
  • 出版日期:2015-04-25 发布日期:2015-04-28
  • 基金资助:

    黑龙江省自然科学基金项目(C201303);黑龙江省教育厅科学技术研究项目(12541045);
    “十二五”国家科技支撑计划项目(2012BAD28B00-01-02)

Determination of Acrylamide in Deep-Fried Pork by Solid Phase Extraction-High Performance Liquid Chromatography

SHAO Meili1, HAO Xingyu1, LIU Wei1,2, CUI Chengyuan1, YUAN Zhaofeng1, DONG Xin1   

  1. 1. College of Food Sciences, Northeast Agricultural University, Harbin 150030, China;
    2. Jiamusi Entry-Exit Inspection and Quarantine Bureau, Jiamusi 154002, China
  • Online:2015-04-25 Published:2015-04-28

摘要:

建立油炸猪肉中丙烯酰胺的固相萃取-高效液相色谱检测方法。油炸猪肉样品经正己烷脱脂,2 mol/L氯化钠溶液提取,乙酸乙酯萃取,固相萃取小柱净化后,以甲醇-水(5∶95,v/v)为流动相,Hypersi10DS2-C18色谱柱分离,内标法定性、定量分析丙烯酰胺。结果表明:丙烯酰胺的定性检出限为6 μg/kg,定量检出限为20 μg/kg,线性定量范围0.05~1.00 μg/mL,线性相关系数(R2)为0.999 8,本方法的加标回收率稳定在90%~92%范围,相对标准偏差小于3.5%。

关键词: 油炸猪肉, 丙烯酰胺, 固相萃取, 高效液相色谱

Abstract:

A method for the determination of acrylamide in deep-fried pork has been proposed using solid phase extraction
(SPE) and high performance liquid chromatography (HPLC). Samples were degreased with n-hexane and extracted
sequentially with 2 mol/L sodium chloride solution followed by ethyl acetate. Then the extract was cleaned up on an Oasis
HLB solid phase extraction column and separated on a Hypersi10DS2-C18 chromatographic column with a mobile phase
consisting of methanol and water (5:95, v/v). Acrylamide was analyzed quantitatively by internal standard method. The
results showed that the limit of qualitative detection of the proposed method was 6 μg/kg, and the limit of quantitative
detection was 20 μg/kg. The standard curve was linear within the range of 0.05–1.00 μg/mL with a correlation coefficient of
0.999 8. The recoveries of the spiked sample ranged between 90% and 92% with a relative standard deviation (RSD) lower
than 3.5%. This method proved to be simple, fast and highly sensitive.

Key words: deep-fried pork, acrylamide, solid-phase extraction, high performance liquid chromatography

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