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基于双水相体系的绿色提取方法用于高效液相色谱-串联质谱定量分析前中药中多残留农药的痕量富集。

A green extraction method based on aqueous two-phase system for trace-level enrichment of multi-residue pesticides in traditional Chinese medicine prior to HPLC-MS/MS quantitative analysis.

机构信息

Department of Chemistry and Chemical Engineering, Hunan Institute of Science and Technology, Yueyang, 414006, PR China; Henan Key Laboratory of Biomarker Based Rapid-detection Technology for Food Safety, Food and Pharmacy College, Xuchang University, Xuchang, 461000, PR China.

Department of Chemistry and Chemical Engineering, Hunan Institute of Science and Technology, Yueyang, 414006, PR China.

出版信息

J Chromatogr A. 2024 Dec 6;1738:465462. doi: 10.1016/j.chroma.2024.465462. Epub 2024 Oct 24.

Abstract

At present, the matrix interference in traditional Chinese medicine (TCM) is still a great challenge for multi-residue pesticides analysis. Herein, an alcohol/salt aqueous two-phase system (ATPS) based on n-propanol and (NH)SO was developed by comparing the binodal curve phase diagrams and the extraction rates of pesticides. The specific extraction conditions, including the composition of the ATPS, temperature, pH, and extraction time were explored through single factor experiments, and subsequently optimized using orthogonal array design and response surface methodology. The optimal conditions for the (NH)SO/n-propanol ATPS extraction were determined to be: extraction time of 30 min, (NH)SO concentration of 22 %, temperature of 62.07 °C, n-propanol concentration of 30.13 %, and pH value of 7.66. In addition, the HPLC-MS/MS quantitative analysis of 25 pesticides in TCMs (i.e., honeysuckle and lily) was accomplished with recovery rates ranging from 64.2 % to 117.1 %. Moreover, the greenness of this method was evaluated using an analytical greenness calculator, and compared with other extraction techniques. The results indicate that the developed method is simple, efficient, and environmentally friendly, capable of trace-level enriching and simultaneously detecting multi-residue pesticides in TCM.

摘要

目前,中药材中基质干扰仍然是多残留农药分析的一大挑战。本研究通过比较双相区相图和农药萃取率,开发了一种基于正丙醇和(NH)SO 的醇/盐双水相体系(ATPS)。通过单因素实验,对包括 ATPS 组成、温度、pH 值和萃取时间在内的具体萃取条件进行了探讨,并进一步通过正交试验设计和响应面法进行了优化。(NH)SO/正丙醇 ATPS 萃取的最佳条件为:萃取时间 30 min、(NH)SO 浓度 22%、温度 62.07°C、正丙醇浓度 30.13%、pH 值 7.66。此外,采用高效液相色谱-串联质谱法(HPLC-MS/MS)对中药材(金银花和百合)中的 25 种农药进行了定量分析,回收率在 64.2%至 117.1%之间。此外,还使用分析绿色计算器对该方法的绿色性进行了评估,并与其他萃取技术进行了比较。结果表明,该方法简单、高效、环保,能够对中药材中的多残留农药进行痕量富集和同时检测。

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