摘要
目的建立奶茶中甜蜜素的甲醇沉淀-气相色谱测定方法。方法样品加甲醇涡旋混合提取后,离心分离,取上清液沸水浴除去甲醇,在硫酸介质中衍生反应,正已烷提取气相色谱分离,氢火焰离子化检测器测定,保留时间定性,外标法定量。结果甜蜜素在0.02 g/kg～0.8 g/kg浓度内线性良好,相关系数(r)为0.999 8,方法检出限为0.001 g/kg,定量限为0.003 g/kg。对奶茶样品进行高、中、低3个浓度加标水平测定,回收率为93.3%～96.0%,相对标准偏差(RSD)为3.97%～4.76%。结论该方法前处理快速简单,沉淀分离效果好,避免了复杂基质的干扰,结果重现性好、准确度高,适合奶茶中甜蜜素的测定。
Objective To establish a method for the determination of sodium cyclamatr in milk tea by methanol precipitation-gas chromatography.Methods The sample was vortex mixing extracted with methanol,then centrifuged.Methanol was removed from the supernatant in boiling water bath.Sodium cyclamate was derivatized in sulfuric acid medium,then extracted with hexane,separated with gas chromatographic,detected by flame ionization detector,qualified by retention time,and quantified by external standard method.Results The method had a good linearity within 0.02g/kg-0.8g/kg,with the correlative coefficient(r)of 0.999 8,the limit of detection was 0.001 g/kg,and the limit of quantification was 0.003 g/kg.The recoveries of milk tea al low,medium and high levels were within 93.3%-96.0%,with the relative standard deviations(RSD)of 3.97%-4.76%.Conclusion The method is simple,rapid,accurate and reproducible,which has good precipitation separation degree,can avoid the interference of complex substrate,and is suitable for the determination of sodium cyclamate in milk tea.
作者
陈国征
王萍
CHEN Guo-zheng;WANG Ping(Tongxiang Center for Disease Control and Prevention,Tongxiang,Zhejiang 314500,China)
出处
《中国卫生检验杂志》
CAS
2019年第7期787-789,共3页
Chinese Journal of Health Laboratory Technology
关键词
甲醇沉淀
气相色谱法
奶茶
甜蜜素
Methanol precipitation
Gas chromatographic
Milk tea
Sodium cyclamate
