高压液相色谱法检测酸性乳饮料及酸奶中对羟基苯甲酸酯类

Determination of p-hydroxybenzoic acid esters in milk and dairy products by high pressure liquid chromatography

中文关键词:  羟基苯甲酸甲酯  对羟基苯甲酸乙酯  对羟基苯甲酸丙酯  对羟基苯甲酸丁酯  高压液相色谱

英文关键词:methyl p-hydroxybenzoic acid ester  ethyl p-hydroxybenzoic acid ester  propyl p-hydroxybenzoic acid ester  butyl p-hydroxybenzoic acid ester  high pressure liquid chromatography (HPLC)

中文摘要:

      目的 建立酸性乳饮料及酸奶中对羟基苯甲酸甲、乙、丙、丁酯含量的高压液相色谱分析方法。方法 样品去蛋白后, 用甲醇提取, 提取液用高压液相色谱仪进行检测。结果 对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯在 0～10 μg/kg 范围内, 相关系数大于 0.999, 检出限分别为 0.48、0.45、0.47、0.49 mg/kg; 在 1、2、5 mg/kg 3 个加标水平下，样品中对羟基苯甲酸甲酯、对羟基苯甲 酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯的加标平均回收率分别为 95.59%~104.52%、93.21%~108.05%、 97.75%~107.98%、97.48%~103.67%, 相对标准偏差均小于 10%。结论 本方法适用于乳与乳制品中对羟基苯 甲酸(尼泊金)甲、乙、丙、丁酯含量的测定需要。

英文摘要:

      Objective To establish a fast and accurate method for determining of methyl p-hydroxybenzoic acid ester, ethyl p-hydroxybenzoic acid ester, propyl p-hydroxybenzoic acid ester and butyl p-hydroxybenzoic acid ester in milk and dairy products by high pressure liquid chromatography(HPLC). Methods After precipitation of protein, the samples were extracted with methanol and the extracts were measured by HPLC. Results A good linear relationship between values of peak area and concentrations of p-hydroxybenzoic acid esters was obtained in the range of 0~10 μg/kg with the correlation coefficient above 0.999. The limits of detection for methyl p-hydroxybenzoic acid ester, ethyl p-hydroxybenzoic acid ester, propyl p-hydroxybenzoic acid ester and butyl p-hydroxybenzoic acid ester were 0.48, 0.45, 0.47, 0.49 mg/kg, respectively and the recoveries were 95.59%~104.52%, 93.21%~108.05%, 97.75%~107.98%, 97.48%~103.67% at three spike level of 1, 2, 5 mg/kg, with relative standard derivations less than 10%, respectively. Conclusion This method can meet the demand for determining of p-hydroxybenzoic acid esters in milk and dairy products.