QuEChERS-离子色谱法测定巴沙鱼中氯酸盐、亚氯酸盐

Determination of chlorate and chlorite in pangasius by QuEChERS-ion chromatography

目的建立巴沙鱼中氯酸盐、亚氯酸盐的QuEChERS-离子色谱检测方法。方法样品经超声提取,经N-丙基乙二胺(PSA)和十八烷基硅烷(C18)净化后,梯度淋洗-抑制型电导检测器离子色谱法检测,外标法定量。结果本方法氯酸盐、亚氯酸盐在0.025~1.000mg/L范围内线性关系良好,相关系数r≥0.9993,氯酸盐最低检测质量浓度为0.15mg/kg,亚氯酸盐最低检测质量浓度为0.50mg/kg。在冷冻巴沙鱼样品中加入3个加标水平下的加标回收率范围为84.4%~101.4%,相对标准偏差(RSD)为1.8%~3.6%。结论建立的方法具有操作简便、分离效果好,灵敏度、精密度和准确度高的特点,适用于巴沙鱼中氯酸盐、亚氯酸盐测定。

Objective To establish a QuEChERS-ion chromatography method for the determination of chlorate and chlorite in Pangasius.Methods The samples were extracted by ultrasonic,purified by N-propyl ethylene diamine(PSA)and octadecyl silane(C18),then detected by gradient elution-suppressed conductivity detector ion chromatography,and quantified by external standard method.Results This method had good linear relationships for chlorate and chlorite mass concentrations in the range of 0.025-1.000 mg/L,the correlation coefficients were greater than 0.9993,the minimum detection concentration of chlorate was 0.15 mg/kg,the minimum detection concentration of chlorite was 0.50 mg/kg.Three spikes were added to frozen pangasius samples,the recovery rates of standard addition at the level ranged from 84.4%to 101.4%,and the relative standard deviation(RSD)was from 1.8%to 3.6%.Conclusion This method has the characteristics of simple operation,good separation effect,high sensitivity,precision and accuracy.It is suitable for the determination of chlorate and chlorite in pangasius.