摘要
目的建立以低共熔溶剂为萃取剂的分散相液相微萃取法,用于测定塑料药品包装材料中5种抗氧剂的迁移。方法四正丁基氯化铵与环己基丙酸按摩尔比1:2,在60℃水浴下搅拌,形成低共熔溶剂。该低共熔溶剂具有疏水性,作为液相微萃取的萃取剂。取该低共熔溶剂与四氢呋喃按体积比5:1的混合液120μl,迅速注入5 ml经预处理的样品溶液中,以2500 r/min涡旋1 min后,形成乳浊液,进行萃取,以8000 r/min离心5 min,使两相分离。取聚集于离心管底部的低共熔溶剂用于高效液相色谱分析。结果5种抗氧剂富集倍数为38倍~74倍,在0.08μg/ml~0.50μg/ml范围内线性良好,相关系数r>0.991,检出限为0.005μg/ml~0.024μg/ml;回收率为93.1%~105.2%,测定值的相对标准偏差(n=6)为2.3%~5.8%。结论该方法制备的低共熔溶剂可作为萃取溶剂,用于液相微萃取法测定塑料药品包装材料中多种抗氧剂在液体样品中的迁移,方法简便、低成本,灵敏度高。
Objective This paper aims to establish a liquid microextraction method with a deep eutectic solvent(DES)as extractant to determine migration of antioxdants from plastic pharmaceutical packaging materials.Methods A deep eutectic solvent was formulated by mixture tetrabutylammonium chloride and cyclohexanepropionic acid at the molar ratio of 1∶2 in a 60℃water bath.This solvent was hydrophobic and used as extractant in liquid microextraction.120μl mixture of DES and tetrahydrofuran(THF)at the volume ration of 5∶1 were quickly injected into 5 ml prepared sample to form an emulsion by the assistance of 1 min vortex agitation at 2500 r/min.Phase separation was carried out by centrifugation at 8000 r/min for 5 min,and the DES at the bottom of the tube was collected and analyzed by high performance liquid chromatography(HPLC).Results The method exhibited enrichment factor values of 5 kinds of antioxdants ranging from 37 to 74.The method showed good linear relationship in the range of 0.08μg/ml-0.50μg/ml,with the correlation coefficients(r)above 0.991,the 1imits of detection(LOD)ranged from 0.005μg/ml to 0.24μg/ml.The recoveries were from 93.1%to 105.2%,with relative standard deviations(RSD)of 2.3%-5.8%(n=6).Conclusion The proposed DES could be used as extractant in liquid phase microextraction for the migration determination of antioxdants from plastic pharmaceutical packaging materials into liquid samples.The feature of the procedure lies in simplicity,low cost and high sensitivity.
作者
刘萌
王晓园
张崇生
李志梅
LIU Meng;WANG Xiao-yuan;ZHANG Chong-sheng;LI Zhi-mei(Wenzhou Research Institute for Food and Drug Control,Zhejiang 325000,China)
出处
《中国卫生检验杂志》
CAS
2023年第20期2456-2459,共4页
Chinese Journal of Health Laboratory Technology
基金
温州市基础性科研项目(Y20211027)。
关键词
低共熔溶剂
液相微萃取
抗氧剂
药品包装材料
Deep eutectic solvent
Liquid phase microextraction
Antioxdants
Pharmaceutical packaging materials
