高效液相色谱法测定起酥油中的苯甲酸和山梨酸

Determination of benzoic acid and sorbic acid in shortening oil by high per-formance liquid chromatography

中文关键词:  高效液相色谱法  起酥油  苯甲酸  山梨酸

英文关键词:high performance liquid chromatography  shortening oil  benzoic acid  sorbic acid

中文摘要:

      目的 建立起酥油中苯甲酸和山梨酸的高效液相色谱法测定方法, 对GB/T 5009.29中没有涉及的食品类型的检测方法进行补充。方法 样品使用弱碱水提取, 用弱酸液体将溶液调至弱酸性(pH约为6), 经过0.2 μm微孔过滤膜过滤; 进样分析。色谱柱: CNW C18色谱柱(250 mm×4.6 mm, 5 μm); 流动相: B相, 甲醇溶液, 5%; C相, 10 mmol/L乙酸铵水溶液(50 mL甲醇+950 mL超纯水, 0.77 g乙酸铵), 95%; 检测波长: 230 nm; 流速: 1.0 mL/min; 柱温: 室温; 进样量: 3.0 μL; 采用色谱峰保留时间定性, 外标法峰面积定量。结果 在1～50 μg/mL范围内线性良好, 苯甲酸和山梨酸的相关系数均大于0.99, 平均回收率93.76%和98.00%, 相对标准偏差9.22%和10.93%, 检出限都是1 mg/kg。结论 该方法具有样品预处理简单、分析速度快、灵敏度高的特点, 可用于起酥油中苯甲酸和山梨酸的同时快速检测。

英文摘要:

      Objective To establish a high performance liquid chromatography method for determination of benzoic acid and sorbic acid in shortening oil, which food type does not involved in GB/T 5009.29 detection ruler. Methods The sample was extracted by weak base water and converted the extraction liquid to weak acidic (pH about 6) with weak acid solution, then the sample was analyzed after filtering with 0.2 μm microfiltration membrane. The detection condition was as column: CNW C18 column (250 mm×4.6 mm, 5 μm); mobile phase: B phase, methanol solution, 5%; C phase, 10 mmol/L ammonium acetate solution (50 mL of methanol +950 mL ultrapure water , 0.77 g ammonium acetate), 95%; detection wavelength: 230 nm; flow rate: 1.0 mL/min; column temperature: room temperature; and injection volume: 3.0 μL. Finally, the benzoic acid and sorbic acid in shortening oil were qualitatively analyzed with chromatographic peak retention time and quantitatively analyzed with external standard peak area, respectively. Results This method showed a good linearity in 1~50 μg / mL (r2>0.99), the average recoveries were 93.76% and 98.00%, and relative standard deviation were 9.22% and 10.93%, and the detection limit was 1 mg /kg. Conclusion The sample preparation method is simple, rapid and high sensitive, which can be used for the rapid detection of benzoic acid and sorbic acid in shortening oil.