摘要
目的对常用食品添加剂糖精钠、山梨酸的假阳性情况进行研究。通过比较紫外检测器和二极管阵列检测器在样品假阳性检测中的应用,确定二极管阵列检测器在排除假阳性方面的重要性。方法称取均匀样品加水,经水浴超声提取20 min后冷却,分别用2 mL亚铁氰化钾和乙酸锌溶液沉淀蛋白,离心后转移水相,残渣进行二次提取,合并上清液后定容,采用高效液相色谱法进行测定。结果糖精钠检测中使用配有紫外检测器的高效液相色谱仪,加标回收率为92%,因此判定该样品为阳性样。经复检,判定为阴性样。山梨酸检测中使用配有二极管阵列检测器的高效液相色谱仪,利用保留时间及光谱信息,确定样品为阳性样,排除假阳性。结论紫外检测器利用保留时间进行定性,食品基质如果有干扰,在目标峰保留时间出峰,就会造成假阳性。而二极管阵列检测器通过全波段扫描,从保留时间、光谱信息、峰纯度等进行综合定性分析,对于基质较复杂的食品样品更能保证结果的准确性。
Objective To study the false-positive of saccharin sodium and sorbic acid additives in food.By comparing the application of UV detector and diode array detector in the detection of false positive samples,the importance of diode array detector in eliminating false positive was determined.Methods Weighed uniform sample and added water,after ultrasonic extraction in water bath for 20 minutes and cool,2 mL of potassium ferricyanide and zinc acetate were used to precipitate the protein.The aqueous phase was transferred after centrifugation and rextracted the residue.The supernatant was combined and diluted to 50 mL volume,and then measured by high performance liquid chromatography.Results The high performance liquid chromatograph with ultraviolet detector was used in the detection of saccharin sodium.The spiked recovery was 92%and the sample was determined to be positive sample.However,it was judged to be a negative sample after retesting.The high performance liquid chromatograph with diode array detector was used in sorbic acid detection.Combined with the retention time and spectral information,the sample was confirmed to be positive and false positive was excluded.Conclusion UV detector uses the retention time for qualitative analysis,if there is interference in the food matrix,the peak will appear at the retention time of the target peak,which will cause false positive.The diode array detector performs comprehensive qualitative analysis from retention time,spectral information,peak purity,etc.Through full wavelength scanning,which can ensure the accuracy of the results of samples with complex food matrix.
作者
毛敏
赵慧明
孙小龙
MAO Min;ZHAO Hui-Ming;SUN Xiao-Long(Yulin Food Inspection and Testing Center,Yulin 719000,China)
出处
《食品安全质量检测学报》
CAS
2020年第14期4829-4835,共7页
Journal of Food Safety and Quality
关键词
高效液相色谱法
二极管阵列检测器
食品添加剂
假阳性
high performance liquid chromatography
diode array detector
food additives
false positive
