发酵乳及果酱中苯甲酸、山梨酸、糖精钠和安赛蜜的高效液相色谱法测定

High Performance Liquid Chromatography Determination of Benzoic Acid, Sorbic Acid, Saccharin Sodium and Acesulfame K in Fermented Milk and Jam

建立发酵乳及果酱中苯甲酸、山梨酸、糖精钠和安赛蜜的反相高效液相色谱分析方法。用水做提取剂,在C18反相色谱柱上进行分离,采用乙酸铵缓冲溶液(20 mmoL/L,pH 4.6)-甲醇为流动相进行等度洗脱,用于苯甲酸和山梨酸测定时流动相A、B的体积比为85∶15,糖精钠和安赛蜜测定时为95∶5,采用紫外检测器在254 nm波长处检测,外标法定量。结果表明:发酵乳样品中苯甲酸、山梨酸、糖精钠和安赛蜜的添加量为1～20 mg/kg时,加标回收率为92.0%～102.4%;果酱样品中苯甲酸、山梨酸、糖精钠和安赛蜜的添加量为5～20 mg/kg时,加标回收率为92.3%～105.8%;发酵乳中苯甲酸、山梨酸、糖精钠和安赛蜜的定量限为1 mg/kg,果酱中苯甲酸、山梨酸、糖精钠和安赛蜜的定量限为5 mg/kg。

An high performance liquid chromatographic(HPLC) method for the determination of four sweeteners and one preservative in fermented milk and jam was developed in this paper. Water was used as the extraction solvent. The chromatographic separation was performed on a reversed phase C18 column using a mobile phase composed of a mixture of 20 mmol/L ammonium acetate buffer solution(pH 4.6) and methanol by isocratic elution. The ratio between mobile phase A and B was 85:15(V/V) for the detection of benzoic acid and sorbic acid and 95:5(V/V) for the detection of saccharin sodium and acesulfame K. The analytes were detected using an ultraviolet detector at 254 nm and quantified by an external standard method. The recoveries for benzoic acid, sorbic acid, saccharin sodium and acesulfame K in fermented milk at spiked levels of 1–20 mg/kg were 92.0%–102.4%, and the recoveries in jam at spiked levels of 5–20 mg/kg were 92.3%–105.8%. The limit of quantification(LOQ) for all analytes was 1 and 5 mg/kg in fermented milk and jam, respectively.