提出了高效液相色谱法测定食品添加剂中水杨酸含量的方法。样品采用含0.1%(体积分数)甲酸的甲醇-水(9+1)混合溶剂溶解,超声提取后经0.22 μm滤膜过滤,滤液供高效液相色谱荧光仪测定。采用ZORBAX SB-C18色谱柱(4.6 mm×250 mm,3.5 μm)分离,用不同配比的(A)甲酸-乙腈(0.1+99.9)和(B)甲酸-水(0.1+99.9)的混合溶液为流动相梯度洗脱,在激发波长为290 nm、发射波长为400 nm处检测。水杨酸的质量浓度在41.60~1 664 μg·L-1范围内与其对应的峰面积呈线性关系,检出限(3S/N)为1.55 μg·L-1,方法的回收率在90.4%~101.7%。

HPLC was applied to the determination of salicylic acid in food additives. The sample was dissolved with mixed solvent of methanol-H2O (9+1) (containing 0.1% formic acid by vol.) and extracted ultrasonically. After filtering on 0.22 μm filtering membrane, the solution was used for HPLC analysis. The ZORBAX SB-C18 chromatographic column (4.6 mm×250 mm, 3.5 μm) was used for separation and a mixture of (A) formic acid-acetonitrile (0.1+99.9) and (B) formic acid (0.1+99.9)solution mixed in different ratio were used as the mobile phase in gradient elution. Fluorimetric detection at the wavelengths of (λex) 280 nm and (λem) 450 nm was adopted. Linear relationship between values of peak area and mass concentration of salicylic acid was obtained in the range of 41.60~1 664 μg·L-1, with detection limit (3S/N) of 1.55 μg·L-1. Values of recovery of the method found were in the range of 90.4%-101.7%.