酱卤肉制品中酸性橙Ⅱ检测方法的优化

冯寅洁; 乔勇升; 纪晨; 陈伟

doi:10.13386/j.issn1002-0306.2017.18.045

酱卤肉制品中酸性橙Ⅱ检测方法的优化

Optimization of the determination of acid orange Ⅱin soy sauce and pot-roast meat products

摘要

摘要: 优化了固相萃取-高效液相色谱检测酱卤肉制品中酸性橙Ⅱ的方法。样品经过石油醚去油后,用氨水-乙醇-水溶液（体积比20∶70∶10）提取,70℃水浴浓缩,调节pH至5⁶,通过Cleanert PWAX弱阴离子交换柱净化和富集,60℃水浴挥干洗脱液后用水溶解定容,借助Thermo Hypersil Gold C₁₈色谱柱（250 mm×4.6 mm,5μm）分离,20 mmol/L乙酸铵溶液-甲醇（体积比35∶65）为流动相,以1 m L/min的流速等度洗脱。结果表明:酸性橙Ⅱ在0.1⁵μg/m L内线性良好,相关系数（r）大于0.99995,检出限为0.01 mg/kg。对鸭翅空白样品分别进行0.5、1.0、1.5、2.0 mg/kg四种水平的加标回收实验,酸性橙Ⅱ的加标回收率为80.8%⁸6.3%,相对标准偏差为2.1%⁴.7%（n=6）。该方法去除了样品中的基质干扰,较好地提取了酸性橙Ⅱ,选用的固相萃取柱净化和富集效果理想,具有灵敏度高、可操作性强、重复性好、适用于批量检测等特点。

Abstract: An optimized method was developed for the determination of acid orangeⅡin soy sauce and pot-roast meat products by HPLC-SPE.Samples were firstly removed oil by petroleum, extracted by ammonia-ethanol-water solution (20∶70∶10 of volume ratio) , concentrated by water bath at 70℃, and adjusted p H value to 5⁶.Then, the extraction was cleaned and enriched by Agela Cleanert WPAX weak anion exchange column.The elution was dried by water bath at 60℃and dissolved with water to a constant volume.Sample solution were separated by Thermo Hypersil Gold