SPE-UPLC-MS/MS测定葡萄酒中的高氯酸盐

为建立前处理简单、定量准确、灵敏度高的葡萄酒中高氯酸盐的快速测定和分析方法,本研究使用酸化甲醇提取葡萄酒样品,最终选择WAX固相萃取柱前处理净化,亲水性聚丙烯滤膜(GHP)过滤,经Phenyl-Hexyl色谱柱分离,以电喷雾离子源(ESI)在多反应监测(MRM)负离子模式下测定葡萄酒中高氯酸盐。结果表明,该方法的检测时间为12 min,检出限和定量限分别为0.15 μg·L^-1和0.5 μg·L^-1,在1、2、5、10和20 μg·L^-1水平的加标回收率介于94.5%~105%之间,相对标准偏差(RSD)小于3.17%。该方法的建立可为葡萄酒生产企业和相关监管部门提供一定的技术支撑。

Determination of Perchlorate in Wine by SPE-UPLC-MS/MS

In order to establish a rapid analysis method for perchlorate in wines with simple pretreatment, accurate quantification and high sensitivity, wine samples were extracted with acidified methanol solution, purified by WAX solid phase extraction column, filtered by hydrophilic polypropylene membrane (GHP), separated by Phenyl-Hexyl column, electrospray ion source in multiple reaction monitoring and detection in negative ion mode to determine perchlorate in wine. The results showed that the detection time was 12 min, the detection limit and limit of quantitation were 0.15 μg·L^-1 and 0.5 μg·L^-1, respectively. The recoveries at spikes of 1, 2, 5, 10 and 20 μg·L^-1 ranged from 94.5% to 105% with the relative standard deviation (RSD) less than 3.17%. The establishment of this method can provide some technical support for the testing of wine producers and relevant regulatory authorities.