肉鸭表皮组织中脱氢枞酸残留的SPE-HPLC检测方法

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。

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

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.