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目的建立操作简便、灵敏度高的高效液相色谱测定卤肉制品中酸性橙Ⅱ的方法。方法样品经均质,取2 g粉碎样品,乙醇震荡提取5 min,提取液经聚酰胺固相萃取柱分离净化。采用C18色谱柱(250 mm×4.6 mm×5μm)分离,以甲醇-乙酸铵溶液梯度洗脱,流速为1 ml/min,设定柱温30℃,进样体积为10μl,二极管阵列检测器检测酸性橙Ⅱ(λ=484 nm)并测定卤肉中酸性橙Ⅱ的含量及加标回收率,并作方法学论证。结果酸性橙Ⅱ在0.1μg/ml~20μg/ml的范围内,线性关系良好,线性方程为y=34.94x-2.697,r=0.9998。酸性橙Ⅱ最低检出浓度为0.08μg/ml。样品添加浓度为0.5 mg/kg~15 mg/kg时,方法回收率为96%~99%,相对标准偏差为3.39%~7.31%。结论用HPLC法检测非法添加于卤肉中的酸性橙Ⅱ的含量,该操作简便,定量准确可靠。
Objective To establish a simple and sensitive HPLC method for the determination of acid orange Ⅱ in stewed meat products. Methods The samples were homogenized, 2 g crushed samples were taken and extracted with ethanol for 5 min. The extracts were separated and purified by polyamide solid-phase extraction column. The sample was separated on a C18 column (250 mm × 4.6 mm × 5 μm) and eluted with a gradient of methanol-ammonium acetate at a flow rate of 1 ml / min. The column temperature was set at 30 ° C and the injection volume was 10 μl. The diode array detector Acid orange Ⅱ (λ = 484 nm) and the determination of acid orange Ⅱ content of meat and spike recovery, and methodological feasibility studies. Results The results showed that the linear relationship between acidic orange Ⅱ and 0.1μg / ml ~ 20μg / ml was linear. The linear equation was y = 34.94x-2.697, r = 0.9998. Acid Orange Ⅱ minimum detectable concentration of 0.08μg / ml. The method recoveries ranged from 96% to 99% and the relative standard deviations (RSDs) ranged from 3.39% to 7.31% at the concentration of 0.5 mg / kg to 15 mg / kg. Conclusion HPLC method was used to detect the content of acid orange Il illegally added in stewed meat. The method is simple, accurate and reliable.