毛细管气相色谱法快速测定鸡粉和鸡精调味料中甜蜜素

Rapid determination of sodium cyclamate in chicken powder and chicken essence seasoning by capillary gas chromatography

通过优化前处理方法和衍生条件,建立一种快速测定鸡粉和鸡精调味料中甜蜜素含量的毛细管气相色谱法。研究结果表明,当硫酸溶液质量浓度由200 g/L提高到500 g/L时,鸡精调味料样品的加标回收率明显提高,而鸡粉调味料样品的加标回收率变化不明显,样品加标回收率范围是80.15%〜94.38%;当硫酸溶液质量浓度从500 g/L以50 g/L的增量逐渐提高时,样品平均加标回收率呈抛物线式增长。与GB 5009.97-2016中第一法气相色谱法相比,本方法重点解决了鸡精、鸡粉样品中甜蜜素测定的关键技术问题,并且快速、准确、回收率高;整个前处理操作均在50 mL离心管中进行,简单、高效,有利于大批量样品的快速检测。

Through the improvement of pretreatment method and derivatization conditions,a gas chromatography method for a rapid determination of sodium cyclamate in chicken powder seasoning and chicken essence was established.The results showed that,when the concentration of sulfuric acid increased from 200 to 500 g/L,the recovery rates of chicken essence samples were significantly improved,but the recovery rate of chicken powder seasoning sample did not improve much,the recovery rate of sample spiking ranged from 80.15%to 94.38%.When the mass concentration of sulfuric acid solution was gradually increased from 500 to 50 g/L,the average spiked recovery rate of the sample increased parabolically.Compared with the first method of gas chromatography in GB 5009.97-2016,this study focused on solving key technical problems in the determination of cyclamate in chicken essence and chicken powder samples.It was fast,accurate with high recovery rate.The pretreatment operation was carried out in a 50 mL centrifuge tube.The steps were relatively simple and efficient.The method in this study is suitable for a rapid detection of large quantity samples.