肉鸭表皮组织中脱氢枞酸残留的SPE-HPLC检测方法  

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

作　　者：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] 

机构地区：[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　　处：《食品科学》2014年第16期101-104,共4页Food Science

基　　金：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)

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。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.

关 键 词：肉鸭 松香 脱氢枞酸 高效液相色谱法 固相萃取 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程] O657.72[轻工技术与工程—食品科学与工程]