Wu Beiqi, Niu Yu, Bi Xinyuan, Wang Xiaowen, Jia Liyan, Jing Xu
College of Food Science and Engineering, Shanxi Agricultural University, Taigu, Shanxi 030801, China.
Agricultural Economics and Management College, Shanxi Agricultural University, Taiyuan, Shanxi 030006, China.
Anal Methods. 2022 Mar 31;14(13):1329-1334. doi: 10.1039/d1ay02130c.
A rapid and convenient analytical procedure (evaporation-assisted dispersive liquid-liquid microextraction with solidification of floating organic droplets) is advanced for determining the concentrations of triazine herbicide residues ( simazine and atrazine) in fruit juices HPLC-DAD. The technique involves adding 1-dodecanol (low density) and dichloromethane (high density) to the test solution to act as the extraction and volatile solvents, respectively. Calcium oxide is added to generate heat to accelerate the evaporation of dichloromethane, whereupon the 1-dodecanol quickly disperses into small droplets to complete the microextraction process. Thus, there is no need to use a dispersive solvent and heating equipment is also not required. The floating 1-dodecanol is subsequently frozen using an ice bath to facilitate its separation from the sample. Under optimal conditions (250 μL of 1-dodecanol (extraction solvent), 150 μL of CHCl (volatile solvent), 1250 mg of CaO, and an extraction time of 60 s) the detection procedure is linear over the range 0.05-5 μg mL (with > 0.99). The limits of detection (LOD) and quantification (LOQ) were determined to be 0.0022-0.0034 μg mL and 0.0073-0.0113 μg mL, respectively. The recovery of simazine and atrazine in three fruit juices ranged between 78.5% and 96.4% with a relative standard deviation <8.2%. Therefore, the proposed approach can be effectively adopted to analyze the triazine herbicide content in fruit juices. The method has been proved to be simple, reliable, and remarkably efficient.
本文提出了一种快速便捷的分析方法(蒸发辅助分散液液微萃取-浮质固化法),用于测定果汁中三嗪类除草剂残留(西玛津和莠去津)的含量,并结合高效液相色谱-二极管阵列检测法(HPLC-DAD)进行分析。该技术是向测试溶液中分别加入1-十二醇(低密度)和二氯甲烷(高密度),作为萃取溶剂和挥发性溶剂。加入氧化钙以产生热量,加速二氯甲烷的蒸发,此时1-十二醇迅速分散成小液滴,从而完成微萃取过程。因此,无需使用分散剂,也不需要加热设备。随后,使用冰浴将漂浮的1-十二醇冷冻,以便于其与样品分离。在最佳条件下(250 μL 1-十二醇(萃取溶剂)、150 μL CHCl(挥发性溶剂)、1250 mg CaO、萃取时间60 s),检测程序在0.05-5 μg/mL范围内呈线性(相关系数>0.99)。检测限(LOD)和定量限(LOQ)分别确定为0.0022-0.0034 μg/mL和0.0073-0.0113 μg/mL。三种果汁中西玛津和莠去津的回收率在78.5%至96.4%之间,相对标准偏差<8.2%。因此,所提出的方法可有效地用于分析果汁中的三嗪类除草剂含量。该方法已被证明简单、可靠且效率显著。