柱前衍生-高效液相色谱法测定馒头中甜蜜素的研究  

Determination of sodium cyclamate in steamed bread by pre-column derivatization-high preformance liquid chromatography

作　　者：姚誉阳[1] 朱鹏飞[1] 戴维杰[1] 吴宇伉 孟元华[1,2] 刘文卫 陆阳[1] YAO Yuyang;ZHU Pengfei;DAI Weijie;WU Yukang;MENG Yuanhua;LIU Wenwei;LU Yang(Wuxi Centre for Disease Control and Prevetion,Jiangsu Provincial Key Laboratory of Food Safety Risk Monitoring(In the Field of Organic Pollutants),Wuxi 214023;Public Health Research Centre,Jiangnan University,Wuxi 214122)

机构地区：[1]无锡市疾病预防控制中心,江苏省食品安全风险监测重点实验室(有机污染物领域),无锡214023 [2]江南大学公共卫生研究中心,无锡214122

出　　处：《中国食品添加剂》2021年第6期97-102,共6页China Food Additives

基　　金：无锡市“科教强卫工程”项目(CXPT(SYS)002);江南大学公共卫生研究中心项目(JUPH201818)。

摘　　要：建立了柱前衍生-高效液相色谱法测定馒头中甜蜜素的方法,优化了衍生化条件、提取条件和色谱条件。最优化的测定条件为:取馒头样品5g,用25mL纯水涡旋振荡提取两次,离心,合并两次提取液,用水稀释至50mL,精确量取10mL进行衍生化。依次加入1.0mL次氯酸钠,2.0mL硫酸和5.0mL正己烷,剧烈振摇1min后静置分层,除去水层后,正己烷层加入25mL碳酸氢钠溶液,取有机相过微孔滤膜待测。色谱柱采用C18柱,流动相比例为乙腈-水(70∶30,V/V),流速1.0mL/mL,进样量10μL,波长314nm。结果显示,甜蜜素在20.0-200μg/mL范围内线性良好,相关系数为0.9999,方法检出限为10mg/kg,定量限为30mg/kg,加标回收率为97.5%-101.2%,RSD为0.67%-0.99%。本方法前处理简便,回收率高,重复性好,定量准确,干扰少,适合于馒头中甜蜜素的检测,与气相色谱法比具有明显优势。A pre-column derivatization-high performance liquid chromatography method for the determination of sodium cyclamate in steamed bread was established,and the derivatization conditions,extraction conditions and chromatographic conditions were optimized.The optimized measurement conditions are:take 5g of steamed bread sample,vortex and extract twice with 25mL of pure water,centrifuge,combine the two extracts,dilute to 50mLwith water,and accurately measure 10mL for derivatization.Add 1.0mL of sodium hypochlorite,2.0mL of sulfuric acid and 5.0mL of n-hexane in sequence,shake vigorously for 1 min and then stand for separation.After removing the water layer,add 25mL of sodium bicarbonate solution to the n-hexane layer,and take the organic phase through a microporous membrane for testing.The chromatographic column adopts a C18 column,the mobile phase ratio is acetonitrile-water(70∶30,V/V),the flow rate is 1.0mL/mL,the injection volume is 10μL,and the wavelength is 314nm.The results show that sodium cyclamate has a good linearity in the range of 20.0-200μg/mL,the correlation coefficient is 0.9999,the detection limit of the method is 10mg/kg,the limit of quantification is 30mg/kg,the recovery of standard addition is 97.5%-101.2%,and the RSD is 0.67%-0.99%.The method has simple pretreatment,high recovery,good repeatability,accurate quantification,and less interference.It is suitable for the detection of sodium cyclamate in steamed bread and has obvious advantages compared with gas chromatography.

关 键 词：柱前衍生 高效液相色谱法 馒头 甜蜜素 

分 类 号：O657.72[理学—分析化学] O629.1[理学—化学]