建立超高效液相色谱方法测定乳及乳制品中柠檬酸的含量.样品经亚铁氰化钾和乙酸锌沉淀,超声提取,低温冷冻离心沉淀蛋白和脂肪,取上清液,Poroshell 120 Aq-C18(4.6 mm×100.0 mm,2.7 μm)分离,以磷酸二氢铵溶液和甲醇为流动相进行梯度洗脱,运用紫外检测器进行检测,外标法定量.结果表明:标准曲线线性良好,相关系数在0.999 9以上,平均加标回收率为95.3%～104.8%,检出限为100 mg/kg,相对标准偏差为0.16%～2.41%.该方法简便、快速、分离效果好,适用于乳及乳制品中柠檬酸的定量分析.
An ultra-high performance liquid chromatography(HPLC)method was established for the determination of the content of citric acid in dairy products.The samples were precipitated by K3Fe(CN)6 and(CH3COO)2Zn,extracted ultrasonically,and cryogenically centrifuged to precipitate protein and fat.The chromatographic separation was accomplished on a Poroshell 120 Aq-C18 column(4.6 mm×100 mm,2.7 μm)using gradient elution with a mobile phase consisting of a mixture of methanol and ammonium dihydrogen phosphate solution.The analyte was detected by an ultraviolet(UV)detector and quantified by the external standard method.The results showed that the calibration curve was linear with a correlation coefficient above 0.999 9.The average recovery from spiked samples was 95.3%-104.8%,the detection limit was 100 mg/kg,and the relative standard deviation(RSD)for precision was 0.16%-2.41%.The method is simple and rapid and has good separation effect.It is suitable for the quantitative analysis of citric acid in milk and dairy products.
徐红;唐振鑫;张雪娇;冀何连;赵姝丽;王忱;高万东;吴晓莉;张彩霞
内蒙古伊利实业集团股份有限公司,内蒙古 呼和浩特 010110
轻工业
柠檬酸;超高效液相色谱;灭菌乳;发酵乳;乳制品
citric acid;ultra-high performance liquid chromatography;sterilized milk;fermented milk;dairy products
《乳业科学与技术》 2023 (006)
40-43 / 4
10.7506/rykxyjs1671-5187-20231011-052
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