可切换亲水溶剂液液微萃取-阳极溶出伏安法检测三乙酸甘油酯中的铅离子  

Switchable hydrophilic solvent liquid-liquid microextraction-anodic stripping voltammetry for determination of lead ions in glyceryl triacetate

作　　者：田雨 张奇 杨钰昆 刘晋利 王珺 褚继登 周利峰 刘永宁 TIAN Yu;ZHANG Qi;YANG Yukun;LIU Jinli;WANG Jun;CHU Jideng;ZHOU Lifeng;LIU Yongning(Shanxi Kunming Tobacco Co.,Ltd.,Taiyuan 030006,China;School of Life Sciences,Shanxi University,Taiyuan 030006,China)

机构地区：[1]山西昆明烟草有限责任公司,太原市小店区030006 [2]山西大学生命科学学院,太原市小店区030006

出　　处：《烟草科技》2024年第12期33-41,共9页Tobacco Science & Technology

基　　金：中国烟草实业发展中心科技项目“电化学传感检测非固态烟用材料中重金属残留的研究”(ZYSYQ-2022-3)。

摘　　要：为了快速测定三乙酸甘油酯样品中铅离子的含量,建立了一种基于可切换亲水溶剂液液微萃取与阳极溶出伏安法联用检测方法。采用可切换亲水性溶剂液液微萃取的方法对三乙酸甘油酯样品进行前处理,研究了萃取剂的缓冲溶液、NaOH添加量、APDC作为螯合剂的使用量以及萃取后的分散剂溶剂体积,建立了一套三乙酸甘油酯的最佳前处理方法;通过新型纳米材料铋纳米粒子修饰丝网印刷电极,开发了用于铅离子检测的电化学传感方法。将二者联用后最终建立了三乙酸甘油酯样品中铅离子残留检测方法。结果表明:①在最佳实验条件下,三乙酸甘油酯中铅离子的线性范围为2~16 mg/kg,线性回归方程为y=0.4115x+3.9572,R^(2)=0.9954,且检出限为0.110 mg/kg。②该阳极溶出伏安法可在5 min内完成对铅离子的检测。③通过对三乙酸甘油酯实际样品的检测,方法的平均回收率在96.5%~99.6%范围内,相对标准偏差在0.79%~3.87%范围内。④将电化学法与原子吸收光谱法以及电感耦合等离子体质谱法比对,证明本方法测定三乙酸甘油酯样品中残留铅离子准确可靠。该方法操作简便、快捷,准确性好,可实现三乙酸甘油酯样品中痕量铅离子的快速和高灵敏检测。A method based on switchable hydrophilic solvent liquid-liquid microextraction and anodic stripping voltammetry was developed for the rapid determination of lead ions in glyceryl triacetate samples.The liquid-liquid microextraction was first used to pretreat glyceryl triacetate samples.The buffer solution of the extractant,the amount of NaOH added,the amount of APDC used as a chelating agent and the solvent volume of the dispersant after extraction were studied,and a series of optimal pretreatment methods for glyceryl triacetate were developed.An electrochemical sensing method for the determination of lead ions was also developed by modifying a screen-printed electrode with bismuth nanoparticles.Finally,a method for the determination of lead ion residues in glyceryl triacetate samples was developed by combining the above two methods.The results showed that:1)Under the optimized experimental conditions,the linear range for the determination of lead ions in glyceryl triacetate samples was 2-16 mg/kg,the linear regression equation was y=0.4115x+3.9572 with R^(2) of 0.9954,and the detection limit was 0.110 mg/kg.2)The anode stripping voltammetry method could realize the determination of lead ions within 5 min.3)The average recoveries and relative standard deviations were 96.5%-99.6%and 0.79%-3.87%,respectively.4)The developed method was accurate and comparable to atomic absorption spectrometry and inductively coupled plasma mass spectrometry for the same determination.This method is simple,fast and accurate,and could rapidly and sensitively determine the trace lead ions in glyceryl triacetate samples.

关 键 词：三乙酸甘油酯 铅离子 阳极溶出伏安法 可切换亲水溶剂 液液微萃取 

分 类 号：TS426[农业科学—烟草工业]