高效液相色谱法测定混合型饲料添加剂中丙酸及丙酸盐含量

Determination of propionic acid and propionate in mixed feed additives by high performance liquid chromatography

建立了液相色谱仪测定混合型饲料添加剂中丙酸及丙酸盐(以丙酸计)的方法。混合型饲料添加剂经去离子水超声提取10 min,过0.45μm滤膜后经C 18液相色谱柱分离,紫外可见检测器在210 nm处定量检测。该方法解决了提取时间、提取溶剂、流动相pH值等关键技术。用该方法测定混合型饲料添加剂时,丙酸的定量限(LOQ)为0.1%。丙酸在混合型饲料添加剂中的含量为0.1%~20.0%时,丙酸的峰面积与质量浓度呈良好的线性关系(R 2≥0.9999),方法回收率为98.7%~102%,相对标准偏差为0.2%~1.2%。该方法操作简单,测定结果准确,可用于混合型饲料添加剂中丙酸及丙酸盐(以丙酸计)测定。

An analytical method was developed for determining propionic acid and propionate(in propionic acid)in mixed feed additives by high performance liquid chromatography.Mixed feed additives were extracted using deionized water for 10 minutes under the ultrasonic assisted condition.After filtration with 0.45μm membrane filter,the samples were separated by a C 18 column.Quantitative measurement was made at 210 nm using ultraviolet-visible detector.Critical contributory factors of determination were discovered,including extraction time,extraction solvent,mobile phase pH.Under the experimental conditions,the limit of quantification(LOQ)for propanoic acid was 0.1%.Good linear relationship(R 2≥0.9999)was obtained between the peak area and mass concentration of propanoic acid when the propanoic acid accounted for 0.1%-20.0%in mixed feed additives.In addition,the method recovery ranged from 98.7%to 102%while the relative standard deviations(RSD)from 0.2%to 1.2%.This method was proven simple,accurate and reliable.It could be applied to the determination of propionic acid and propionate(in propionic acid)in mixed feed additives.