高效液相色谱法测定市售辣条中的苯甲酸和山梨酸

Determination of Benzoic acid and Sorbic Acid in Spicy Strip by HPLC

为建立辣条中的苯甲酸和山梨酸含量的高效液相色谱测定方法。样品经前处理后以亚铁氰化钾溶液和乙酸锌溶液提取,使用YMC-PACK ODS AQ色谱柱(4.6 mm×250 mm,5μm)、在流动相为乙酸铵∶甲醇体积比为95∶5的混合液、流速1.0 mL·min^-1、波长230 nm条件下测定。结果显示:苯甲酸和山梨酸线性相关系数r2均大于0.999,苯甲酸回收率区间为89.02%~137.20%,相对标准偏差RSD区间为0.082%~0.164%,检出限为0.000 055 g·kg^-1;山梨酸的回收率区间为92.90%~102.54%,RSD区间为0.031%~0.920%,检出限为0.000 012 g·kg^-1;实际抽检结果显示市售辣条产品不合格率高达66.7%。本方法具有重现性好、精确度高等优点,适合应用于辣条类产品中苯甲酸和山梨酸的同时定量测定。

To establish a HPLC method for the determination of benzoic acid and sorbic acid in hot strip. The sample was extracted with potassium ferrocyanide solution and zinc acetate solution after pretreatment. Then using PACK-ODS AQ column(4.6 mm×250 mm, 5 μm), under the circumstance that mobile phase is ammonium acetate and methanol mixed liquids(95 ∶ 5, V/V), flow rate of 1.0 ml/min, wavelength of 230 nm. The results show that the linear correlation coefficient r^2 of benzoic acid and sorbic acid is both greater than 0.999, the recovery range of benzoic acid is 89.02% ~ 137.20%, the RSD range is 0.082 ~ 0.164%, and the detection limit is 0.000 055 g/kg;The recovery range of sorbic acid is 92.90% ~ 102.54%, the RSD range is 0.031% ~ 0.92%, and the detection limit is 0.000 012 g/kg. The actual spot check results show that the unqualified rate of hot strip products on the market is as high as 66.7%. This method has the advantages of good reproducibility and high accuracy, and is suitable for the simultaneous quantitative determination of benzoic acid and sorbic acid in spicy products.