高效液相色谱法测定黄酒中苯甲酸、山梨酸和糖精钠含量

Determination of benzoic acid, sorbic acid and saccharin sodium in rice wine by high performance liquid chromatography

中文关键词:  高效液相色谱法  黄酒  食品防腐剂  苯甲酸  山梨酸  糖精钠

英文关键词:high performance liquid chromatography  rice wine  food additives  benzoic acid  sorbic acid  saccharin sodium

中文摘要:

      目的 建立高效液相色谱法测定黄酒中苯甲酸、山梨酸和糖精钠的分析方法。方法 样品经称取、加热、定容, 利用高效液相色谱法检测, 甲醇水混合溶液作为流动相, PDA检测器检测, 苯甲酸、山梨酸和糖精钠的检测波长为230 nm。结果 苯甲酸和山梨酸在0.05~0.30 mg/mL、糖精钠在0.0025~0.0125 mg/mL时, 都具有良好的线性关系, 相关系数(r)均＞0.999。苯甲酸、山梨酸和糖精钠的LOD分别为1.8、1.2、0.1 g/kg, LOQ分别为5.4、3.6、0.3 mg/kg。平均加标回收率为95.1%~96.4%, RSD为2.6%~3.8%。50份黄酒样品中, 苯甲酸检出有19份, 检出率为38.0%, 检测结果范围为0.0025~1.48 g/kg; 山梨酸检出有6份, 检出率为12.0%, 检测结果范围为0.028~0.44 g/kg; 糖精钠检出有24份, 检出率为48.0%, 检测结果范围为0.005~0.73 g/kg。结论 该方法灵敏度高, 回收率高, 检测限低, 符合分析要求, 适合黄酒中苯甲酸、山梨酸和糖精钠的检测要求。

英文摘要:

      Objective To establish a method for the determination of benzoic acid, sorbic acid and saccharin sodium in rice wine by high performance liquid chromatography (HPLC). Methods The samples were weighed, heated and fixed, then detected by HPLC with methanol water mixed solution as mobile phase, with PDA detector, and the detection wavelengths of benzoic acid, sorbic acid and saccharin sodium were 230 nm. Results There were good linear relationships within 0.05~0.30 mg/mL for benzoic acid and sorbic acid, and 0.0025~0.0125 mg/mL for saccharin sodium, with the correlation coeffectients (r)＞0.999. The LODs of benzoic acid, sorbic acid and saccharin sodium were 1.8, 1.2 and 0.1 mg/kg, and the LOQs were 5.4, 3.6 and 0.3 mg/kg, respectively. The average spiked recoveries were 95.1%~96.4%, and the relative standard deviations (RSDs) were 2.6%~3.8%. Among 50 rice wine samples, there were 19 samples of benzoic acid, 6 samples of sorbic acid and 24 samples of saccharin sodium detected, with the detection rates of 38%, 12.0% and 48.0%, and the detection range were 0.0025~1.48, 0.028~0.44 and 0.005~0.73 g/kg, respectively. Conclusions The established method has high sensitivity, high recovery rate, and low detection limit, which is suitable for the detection of benzoic acid, sorbic acid and saccharin sodium in rice wine.