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超声辅助分散液液微萃取-高效液相色谱法快速测定环境水中马兜铃酸

Rapid Determination of Aristolochic Acids in Environmental Water Using Ultrasonic-assisted Dispersive Liquid-Liquid Microextraction Coupled with High Performance Liquid Chromatography

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【作者】 张朝辉陈应庄郭宾陈波马铭

【Author】 ZHANG Zhao-Hui;CHEN Ying-Zhuang;GUO Bin;CHEN Bo;MA Ming;Key Laboratory of Phytochemical R&D of Hunan Province and Key Laboratory of Chemical Biology & Traditional Chinese Medicine Research(Ministry of Education of China),Hunan Normal University;Hunan Biological and Electromechanical Polytechnic;

【通讯作者】 陈波;马铭;

【机构】 湖南师范大学,植化单体开发与利用湖南省重点实验室,化学生物学及中药分析教育部重点实验室湖南生物机电职业技术学院

【摘要】 建立了超声辅助分散液液微萃取(US-DLLME)-高效液相色谱(HPLC)法测定环境水样中马兜铃酸Ⅰ(AA-Ⅰ)和马兜铃酸Ⅱ(AA-Ⅱ)的方法。考察了萃取溶剂和分散剂的种类及用量、超声时间、料液相pH值和盐效应对AA-Ⅰ和AA-Ⅱ富集因子的影响。在最佳萃取条件下,AA-Ⅰ和AA-Ⅱ的富集因子高达95.9和93.4。本方法检测AA-Ⅰ和AA-Ⅱ的线性范围均为0.01~2.00μg/mL,相关系数(R2)分别为0.9994和0.9997,检出限(LOD)分别为2.5和3.0 ng/mL,定量限(LOQ)分别为8.0和9.5 ng/mL。本方法简单、快速,前处理过程仅需12 min。采用本方法对浏阳河水样和湘江水样进行检测,加标回收率在91.7%~97.8%之间,相对标准偏差(RSD)均小于5.7%。本方法环境友好、灵敏度高,适用于环境水样中AA-Ⅰ和AA-Ⅱ的快速测定。

【Abstract】 A novel method was developed for analysis of aristolochic acid Ⅰ and Ⅱ(AA-Ⅰ and AA-Ⅱ) in environmental water by ultrasonic-assisted dispersive liquid-liquid microextraction(US-DLLME) coupled with high performance liquid chromatography(HPLC). The effects of kinds of the extraction solvent and the disperser solvent, the volumes of the extraction solvent and the disperser solvent, the ultrasonic time, the pH value and salt addition in the feed solution on enrichment factor were investigated. Under the optimal extraction conditions, the enrichment factors of up to 95.9 for AA-Ⅰ and 93.4 for AA-Ⅱ were obtained. The established method showed good linearity for both AA-Ⅰ and AA-Ⅱ in the concentration range from 0.01 to 2.00μg/mL with correlation coefficients(R2) of 0.9994 and 0.9997, respectively. The limits of detection(LODs) were 2.5 and 3.0 ng/mL, and the limits of quantitation(LOQs) were 8.0 and 9.5 ng/mL for AA-Ⅰ and AA-Ⅱ, respectively. The pretreatment procedure was completed within 12 min. The recoveries of AA-Ⅰ and AA-Ⅱ in spiked samples were from 91.7%to 96.9% with relative standard deviations(RSDs) less than 5.7% for Liuyang River samples. The recoveries of AA-Ⅰ and AA-Ⅱ in spiked samples were from 91.9% to 97.8% with RSDs less than 5.1% for Xiangjiang River samples. The results demonstrated that the proposed method was sensitive, fast and environmental-friendly, and could be suitable for analysis of AA-Ⅰ and AA-Ⅱ in environmental water.

【基金】 国家自然科学基金项目(Nos.22276050,22276049);湖南省自然科学基金项目(No.2022JJ60070);湖南省教育厅科学研究项目(No.21C1266)资助~~
  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2023年11期
  • 【分类号】X832;O657.72
  • 【下载频次】79
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