离子色谱-电导法检测格瓦斯中痕量溴酸盐  

Determination of trace bromate in Kvass by ion chromatography with conductivity detection

作　　者：邹沫君 吴丽 王正 ZOU Mojun;WU Li;WANG Zheng(Leshan Center for Food and Drug Control,Leshan 614000,China)

机构地区：[1]乐山市食品药品检验检测中心,四川乐山614000

出　　处：《中国酿造》2022年第11期223-227,共5页China Brewing

基　　金：国家市场监督管理总局科技计划项目(2020MK093)。

摘　　要：该研究建立了用离子色谱-电导检测法测定格瓦斯中痕量溴酸盐的分析方法。试样经石油醚洗去油脂,用超纯水振摇提取,依次过0.22μm微孔滤膜、Dionex OnGuard Ⅱ RP小柱及Dionex OnGuard Ⅱ Ag/H小柱处理后进样检测,选用IonPac AS19阴离子交换分离柱,8~45 mmol/L KOH淋洗液梯度洗脱,流速1.0 m L/min,采用抑制型电导检测器检测。结果表明,溴酸盐在1.0~100.0μg/L质量浓度范围内线性良好,相关系数R2为0.999 8;精密度试验结果相对标准偏差(RSD):保留时间RSD为0.21%、峰面积RSD为0.44%;方法检出限(LOD)为0.048μg/g,定量限(LOQ)为0.16μg/g;在2.5μg/L、5.0μg/L、25.0μg/L三个质量浓度添加水平下,平均加标回收率为93.08%~98.05%。该方法精密度、准确性和稳定性良好,操作简便,适用于格瓦斯中痕量溴酸盐检测。A new method for the determination of trace bromate in Kvass by ion chromatography with conductivity detection was established. The samples were washed with petroleum ether to remove oil, extracted by shaking with ultra-pure water, injected and determined after treatment with0.22 μm microporous filter membrane, Dionex On Guard Ⅱ RP column and Dionex OnGuard Ⅱ Ag/H column. IonPac AS19 anion exchange separation column was selected. Gradient elution with 8-45 mmol/L KOH eluent was performed at a flow rate of 1.0 ml/min and detected by inhibitory conductance detector. The results showed that the bromate had good linearity in the mass concentration range of 1.0-100.0 μg/L, the correlation coefficient R2was 0.999 8. The relative standard deviation(RSD) of precision test results was as follows: RSD of retention time 0.21% and RSD of peak area0.44%. The limit of detection(LOD) of the method was 0.048 μg/g, and the limit of quantification(LOQ) was 0.16 μg/g. At the 3 addition levels of mass concentration 2.5 μg/L, 5.0 μg/L and 25.0 μg/L, the average standard recovery rate was 93.08%-98.05%. The method had good precision, accuracy and stability, and was easy to operate, which was suitable for the determination of trace bromate in Kvass.

关 键 词：离子色谱 电导检测器 格瓦斯 溴酸盐 

分 类 号：O658[理学—分析化学]