聚酰胺粉吸附-高效液相色谱法测定蜜饯中合成着色剂

Determination of synthetic colorants in preserved fruit by polyamide adsorption-HPLC

目的建立一种操作简便、结果准确可靠的蜜饯中合成着色剂的检测方法。方法利用纯水直接60℃水浴振摇,4 000 r/min高速离心15 min,数次提取合成着色剂,合并提取液用柠檬酸溶液调节p H后进行聚酰胺粉吸附,甲醇-甲酸混合溶液洗涤,纯水洗到中性后用乙醇-氨水-水混合溶液解吸,80℃水浴浓缩近干,定容后经滤膜过滤进行高效液相色谱仪梯度洗脱,480 nm测定。结果测定合成着色剂峰面积与含量在1μg/ml^50μg/ml浓度时呈良好的线性关系,相关系数r均>0.999 9,测定相对标准偏差(RSD)均<5%,回收率为85.34%~99.13%。结论该方法操作简便、灵敏、结果准确可靠,适合基层实验室开展。

Objective To establish a simple, accurate and reliable determination method of syhthetic colorants in preserved fruit. Methods The sample was shaken in 60℃ water bath with pure water directly and syhthetic colorants were extracted for several times after centrifugation at the speed of 4 000 r/min in 15 min. The pH value of the extracted liquid was regulated with citric acid solution after it was merged. Syhthetic colorants were absorbed with polyamide powder and washed with methanol and formic acid solution. They were absorbed with alcohol - ammonia - water mixed solution in neutral state. Syhthetic colorants were analysed at 480 nm with HPLC gradient elntion after they were concentrated in 80 ~C water bath and filtered with mem- brane. Results The method offered a good linearity among 1 μg/ml - 50 μg/ml and the relation coefficents of them were more than 0.999 9. Relative standard deviations（RSD） were less than 5% and the recovery rates ranged from 85.34% to 99.13%. Conclusion The method is suitable for the analysis of syhthetic colorants in preserved fruit in basic laboratories with simplici- ty, accuracy, sensitivity and reliability.