高效液相色谱法测定预制菜中防腐剂含量

Determination of preservative content in pre-made meals by high performance liquid chromatography

中文关键词:  高效液相色谱  定性确证  食品防腐剂

英文关键词:high performance liquid chromatography  qualitative confirmation  food preservatives

中文摘要:

      目的 建立高效液相色谱法同时检测食品中苯甲酸、山梨酸、脱氢乙酸的方法。方法 样品中加入氢氧化钠溶液超声提取, 经亚铁氰化钾和乙酸锌溶液沉淀蛋白, 用Agilent XDB-C18 (4.6 mm×250 mm, 5 μm)色谱柱进行分离, 流动相为乙酸铵溶液和甲醇(93:7, V:V), 流速为1 mL/min, 柱温为30 ℃, 二极管阵列检测器检测, 检测波长为230 nm和293 nm。同时用二极管阵列检测器分别采集标准溶液和样品溶液的光谱图, 通过比较标准和样品溶液中目标峰的光谱图, 进一步对样品进行定性确证。结果 3种防腐剂在0.5~100.0 mg/L范围内线性关系良好, 相关系数(r)≥0.9994, 检出限为1.7 mg/kg, 定量限为5.0 mg/kg, 平均加标回收率为92.0%~104.0%, 相对标准偏差为0.1%~1.6%。结论 该方法简单、快速、重现性好、回收率高, 适用于预制菜中苯甲酸、山梨酸和脱氢乙酸3种防腐剂的快速检测。

英文摘要:

      Objective To establish a method for the simultaneous detection of benzoic acid, sorbic acid and dehydroacetic acid in pre-made meals by high performance liquid chromatography. Methods Sodium hydroxide solution was added to the sample for ultrasonic extraction. Protein was precipitated with potassium ferrocyanide and zinc acetate solution. Separation was carried out using an Agilent XDB-C18 (4.6 mm×250 mm, 5 μm) chromatographic column. The mobile phase was ammonium acetate solution and methanol (93:7, V:V), with a flow rate of 1 mL/min and a column temperature of 30 ℃. The detection was carried out by a diode array detector with detection wavelengths of 230 nm and 293 nm. At the same time, the spectra of the standard solution and the sample solution were collected respectively by a diode array detector. By comparing the spectra of the target peak in the standard and sample solutions, the samples were further qualitatively confirmed. Results The 3 kinds of preservatives had a good linear relationship within the range of 0.5–100.0 mg/L, with correlation coefficients (r) greater than or equal to 0.9994. The limits of detection were 1.7 mg/kg, the limits of quantitation were 5.0 mg/kg, the recovery rates were 92.0%–104.0%, and the relative standard deviations were 0.1–1.6%. Conclusion This method is simple, rapid, has good reproducibility and high recovery rate, and is suitable for the rapid detection of 3 kinds of preservatives, namely benzoic acid, sorbic acid and dehydroacetic acid in pre-made meals.