邹沫君
(乐山市食品药品检验检测中心,四川 乐山 614000)
摘要:建立用离子色谱/电导检测法测定乳制品中的微量碘的分析方法。试样经乙酸沉淀蛋白,NaOH 洗去脂肪,超声波、涡旋振摇提取,离心分离后,依次过Dionex OnGuard II RP 小柱、0.22μm 微孔滤膜处理后进样检测,选用IonPac AS19 阴离子交换分离柱,在线产生40mmol/L~70mmol/L KOH 淋洗液梯度洗脱,流速1.0mL/min,以抑制型电导检测器检测。结果表明:碘I-在0.0μg/L~200μg/L 质量浓度范围内具有良好的线性关系,相关系数为0.9998;方法检出限为0.055mg/kg;在0.12、0.24、1.20mg/kg 三个添加浓度水平下,平均回收率为91.42%~97.88%。该方法线性范围广,专属性强,准确性和精密度良好,操作较简便,可用于乳制品中碘离子的含量检测。
关键词:离子色谱;电导检测;乳制品;碘离子
Determination of Micro Amounts of Iodide Ion in Dairy Products by Ion Chromatography
ZOU Mo-jun
(Leshan Center for Food and Drug Control,Leshan 614000,China)
Abstract: A new method was established to determine micro amounts of iodide ion in dairy products by ionchromatography with conducting detection. Acetic acid was applied for protein precipitation of samples. The fat waswashed away from samples with sodium hydroxide. Ultrasonic wave method and vortex vibration method was appliedfor extraction. The samples were separated by centrifugation,then filtrated with Dionex OnGuard II RP column and0.22μm membrane. The samples of solution were injected and analyzed. IonPac AS19 was selected as the separationcolumn. The gradient 40mmol/L~70mmol/L KOH solution with a flow rate 1.0mL/min was used as eluents. Autogeneratedconducting detection ASRS ULTRA II 4mm was used. The results showed that the linear relation ofperchlorate was good in the range of 0.0μg/L~200μg/L(r=0.9998). The detection limit was 0.055mg/kg. At theconcentration addition levels of 0.12,0.24 and 1.20mg/kg,the average recovery rates were 91.42%~97.88%. Themethod had a wide linear range,strong exclusivity,good repeatability and accuracy,which is suitable for thequantitative detection of iodide ion in dairy products.
Key words: ion chromatography;conductivity detection;dairy products;iodide ion
中图分类号:TS20 文献标志码:A 文章编号:1007-7871(2023)02-0020-05
2023,Vol.26,No.2