摘要
目的 建立饮料中痕量柠檬黄的检测方法。方法 以β-环糊精/壳聚糖复合物(CDCS)为固相萃取吸附剂,联用高效液相色谱仪进行检测。考察样品pH、萃取时间、吸附剂用量和洗脱剂等条件对萃取柠檬黄效率的影响。结果 CDCS对柠檬黄最大吸附容量为39.1 mg/g,在多次循环使用后吸附容量为最大时的93.0%。在样品溶液pH=6、萃取时间为14 min、CDCS吸附剂用量为15 mg、1 mL 5%盐酸-甲醇作为洗脱剂条件下,饮料中柠檬黄在10~150μg/L范围内线性关系良好,线性方程y=90.57x-4.393,相关系数r为0.999 9,检出限为2μg/L,实际样品的回收率为88.9%~110%,相对标准差(RSD)为0.67%。结论 建立的方法操作简便,绿色环保,可应用于实际样品的检测。
Objective To develop an assay for determination of trace citrine in beverages.Methods Theβ-cyclodextrin/chitosan composites(CDCS)were used as an adsorbent for solid phase extraction,and pipette tip solid phase extraction coupled with high-performance liquid chromatography was employed for determination of trace citrine in beverages.In addition,the effects of sample pH,extraction time,usage of adsorbents and eluent on the extraction efficiency were examined.Results The maximum adsorption ca-pacity of CDCS was 39.1 mg/g,and the maximum adsorption capacity remained 93.0%following muliple cycles of uses.If the sample pH was 6,extraction time was 14 min,the use of CDCS was 15 mg and 1 mL 5%HCl-methanol was used as an eluent,citrine presented a high linear relationship at mass concentrations of 10 to 150μg/L in beverages(r=0.9999),the linear formation was y=90.57x-4.393,with a 2μg/L limit of detection,88.9%to 110%recovery rates of real samples,and a relative standard deviation of 0.67%.Conclusions The established CDCS-based pipette tip solid phase extraction coupled with high-performance liquid chromatography is easy to perform and environment-friendly,which is feasible for detection of real samples.
作者
王露
宋鑫
冯晓青
张敏会
王芹
杨鹏飞
WANG Lu;SONG Xin;FENG Xiao-qing;ZHANG Min-hui;WANG Qin;YANG Peng-fei(Huai'an Municipal Center for Disease Control and Prevention,Huai'an,Jiangsu 223001,China)
出处
《江苏预防医学》
CAS
2023年第5期517-520,共4页
Jiangsu Journal of Preventive Medicine
基金
淮安市科技计划项目(HAB202222)
淮安市突发公共卫生事件应急检测重点实验室(HAP201906)
淮安市突发公共卫生事件应急检测重点实验室培优课题项目(ETPHI-P-14)
淮安市“天医星”医学检验重点实验室(HAP202004)
2017年淮安市科技计划(指导性)项目(HABZ201732)。
关键词
β-环糊精/壳聚糖复合物
柠檬黄
管尖固相萃取
高效液相色谱
β-cyclodextrin/chitosan composites
Citrine
Pipette tip solid phase extraction
High-performance liquid chromatography
