摘要
实验建立快速溶剂提取结合在线固相萃取法提取、净化土壤中依匹噻嗪等7种噻嗪类利尿剂UPLCMS/MS仪定量的检测方法。随机选取代表性土壤样品约1 kg,缩分后自然风干,过100目筛网;准确称取上述土壤样品10.0 g,置全自动加速溶剂萃取仪萃取池中,加硅藻土15.0 g,混合均匀后,按照程序提取;取上述提取液20 mL,以0.1%甲酸溶液(溶剂为甲醇)为流动相A,乙腈为流动相B,按程序洗脱,洗脱液上UPLCMS/MS定性、定量检测。依匹噻嗪、苄氟噻嗪、氢氟噻嗪、三氯噻嗪、氢氯噻嗪、甲氯噻嗪和环戊噻嗪在0.004-4.0μg·mL^(-1)范围内均有良好的线性;检测限分别为0.13、0.18、0.14、0.15、0.28、0.09和0.15μg/kg;方法加标回收率和重复性均符合要求。此方法简单、快速、准确,将利尿剂的污染问题延伸到土壤中,有助于在利尿剂传递的重要环节控制利尿剂的污染问题。
A quantitative method for extraction and purification of 7 thiazide diuretics such as epiziazide in soil by UPLC-MS/MS was established.Representative soil sample of about 1 kg was randomly selected,which was shrunk and dried naturally and passed through a 100-mesh screen.The above 10.0 g soil sample was accurately weighed and placed in the extraction tank of automatic accelerated solvent extractor,and 15.0 g diatomaceous earth was added,mixed evenly,and extracted according to the program;20 mL of the above extraction solution was taken,and the solvent was 0.1%formic acid solution(methanol)as mobile phase A and acetonitrile as mobile phase B.The eluent was eluted according to the program,and the eluent was tested qualitatively and quantitatively by UPLC-MS/MS.Epithiazide,benzofluthiazide,hydrofluthiazide,triclothiazide,hydrochlorothiazide,meclothiazide and cyclopenthiazide have good linearity in the range of 0.004-4.0μg·mL^(-1).The detection limits were 0.13、0.18、0.14、0.15、0.28、0.09 and 0.15μg·kg^(-1),Respectively.The recovery rate and repeatability of the method met the requirements.This method is simple,fast,and accurate,extending the pollution problem of diuretics to the soil,controlling the pollution problem of diuretics in the important link of diuretic transmission,and effectively protecting the environment we rely on for survival.
作者
邓鹂
Deng Li(Yancheng Dafeng Ecological Environment Monitoring Station,Yanchen 224100,China)
出处
《化学研究与应用》
北大核心
2025年第3期718-725,共8页
Chemical Research and Application
