食品科学

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肉鸭表皮组织中脱氢枞酸残留的SPE-HPLC检测方法

张苏珍1,2,耿志明2,*,王道营2,诸永志2,刘 芳2,张牧焓2,卞 欢2,徐为民2   

  1. 1.南京农业大学 肉品加工与质量控制教育部重点实验室,江苏 南京 210095;
    2.江苏省农业科学院农产品加工研究所,江苏 南京 210014
  • 出版日期:2014-08-25 发布日期:2014-08-25
  • 通讯作者: 耿志明
  • 基金资助:

    国家自然科学基金青年科学基金项目(31101312);江苏省农业科技自主创新资金项目(CX(13)3081)

Development of SPE-HPLC Method for Determination of Dehydrogenated Abietic Acid Residue in Duck Skin Tissue

ZHANG Su-zhen1,2, GENG Zhi-ming2,*, WANG Dao-ying2, ZHU Yong-zhi2, LIU Fang2, ZHANG Mu-han2, BIAN Huan2, XU Wei-min2   

  1. 1. Key Laboratory of Meat Processing and Quality Control, Ministry of Education, Nanjing Agricultural University,
    Nanjing 210095, China; 2. Institute of Agricultural Products Processing, Jiangsu Academy of Agricultural Sciences, Nanjing 210014, China
  • Online:2014-08-25 Published:2014-08-25
  • Contact: GENG Zhi-ming

摘要:

建立经松香脱毛处理的肉鸭表皮组织中残留脱氢枞酸的固相萃取-高效液相色谱检测方法。肉鸭表皮组织中的脱氢枞酸用乙腈提取,经C18固相萃取小柱净化,以0.003 mol/L磷酸溶液-甲醇(13∶87,v/v)为流动相,采用反相C18(250 mm×4.6 mm,5 μm)色谱柱分离,以紫外检测器(检测波长212 nm)进行检测。结果表明:该方法检测脱氢枞酸线性范围为0.1~10 mg/L,检测限为0.10 μg/g,定量限为0.33 μg/g。在低中高3 个添加量范围内回收率为80.8%~91.8%。实际样品分析显示,肉鸭表皮中脱氢枞酸含量最高达10.06 μg/g。所建立的分析方法简便快捷、具有较好的灵敏度和可靠性,可用于肉鸭表皮组织中脱氢枞酸残留量的分析。

关键词: 肉鸭, 松香, 脱氢枞酸, 高效液相色谱法, 固相萃取

Abstract:

A high-performance liquid chromatographic (HPLC) method was established to determine dehydrogenated abietic
acid in duck skin. Dehydrogenated abietic acid in duck skin sample was extracted with acetonitrile, followed by purification
with a C18 solid-phase extraction (SPE) cartridge, and detected by HPLC-ultraviolet detector (UV). The chromatographic
conditions were as follows: column, reversed-phase C18 (250 mm × 4.6 mm, 5 μm); mobile phase, a mixture of 0.003 mol/L
phosphoric acid-methanol (13:87, V/V); flow rate, 1.0 mL/min; and detection wavelength, 212 nm. Results indicated that
the linearity ranged from 0.1 to 10.0 mg/L, and the detection limit and the quantification limit were 0.10 μg/g and 0.33 μg/g,
respectively. The recoveries of dehydrogenated abietic acid spiked at 0.5–20 μg/g were in the range of 80.8%–91.8%. The
method was successfully applied for the determination of dehydrogenated abietic acid in rosin-defeathered duck skin, and
the result indicated that content of dehydrogenated abietic acid in the duck sample could reach 10.06 μg/g. The present
method proved to be of high maneuverability and excellent sensitivity and accuracy, and could be employed to analyze
dehydrogenated abietic acid residue in duck skin tissue.

Key words: duck, rosin, dehydrogenated abietic acid, high-performance liquid chromatographic (HPLC), solid polymer electrolyte (SPE)

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