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Combination of gel-electromembrane extraction with switchable hydrophilicity solvent-based homogeneous liquid-liquid microextraction followed by gas chromatography for the extraction and determination of antidepressants in human serum, breast milk and wastewater.
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2020-03-12 , DOI: 10.1016/j.chroma.2020.461041
Majid Behpour 1 , Saeed Nojavan 1 , Sakine Asadi 1 , Ali Shokri 1
Affiliation  

The current study presents for the first time a combination of the gel electromembrane extraction (GEL-EME) and switchable hydrophilicity solvent-based homogeneous liquid-liquid microextraction (SHS-HLLME) methods which can be used as an efficient hyphenated extraction procedure. This coupled method, which was followed by GC-FID, was applied for quantification of antidepressants (desipramine, clozapine, and citalopram) in biological and wastewater samples. The effective parameters of both GEL-EME and SHS-HLLME procedures were optimized. Using an agarose gel membrane, analytes were extracted from 7.0 mL of the sample solution to 500 µL of the aqueous acceptor solution. The maximum extraction of analytes of interest was obtained under the optimized conditions (pH of acceptor solution, 5.0; pH of gel membrane, 5.0; pH of sample solution, 7.0, voltage value, 30 V; and extraction time, 30 min). Then, the acceptor solution was transferred to the extraction cell and the SHS-HLLME procedure was conducted again under the optimized conditions. Dipropylamine (50 µL) was selected as an extraction solvent. The introduced technique exhibited good linearities with coefficients of determinatin (R2) higher than 0.983 and an acceptable linear range of 5.0-1000 ng/mL. Accordingly, the limit of detection was ≤ 1.0 ng/mL (S/N = 3) for all analytes, and the high enrichment factors were obtained in the range of 178.7-194.8. Moreover, the corresponding repeatability was from 4.0 to 8.7% (n = 3). The proposed method was successfully utilized to determine trace levels of the drugs in human serum, wastewater, and breast milk samples.

中文翻译:

凝胶-电膜萃取与可切换亲水性基于溶剂的均相液-液微萃取相结合,然后进行气相色谱法萃取和测定人血清,母乳和废水中的抗抑郁药。

当前的研究首次提出了凝胶电膜萃取(GEL-EME)和可切换亲水性基于溶剂的均相液-液微萃取(SHS-HLLME)方法的组合,可将其用作高效的联用萃取方法。该耦合方法随后是GC-FID,适用于定量生物和废水样品中的抗抑郁药(地昔帕明,氯氮平和西酞普兰)。优化了GEL-EME和SHS-HLLME程序的有效参数。使用琼脂糖凝胶膜,将分析物从7.0 mL样品溶液中萃取到500μL受体水溶液中。在最佳条件下(受体溶液的pH为5.0;凝胶膜的pH为5.0;样品溶液的pH为7.0;电压值30 V; 提取时间30分钟)。然后,将受体溶液转移到萃取池中,并在最佳条件下再次进行SHS-HLLME程序。选择二丙胺(50 µL)作为萃取溶剂。引入的技术表现出良好的线性,测定素(R2)的系数高于0.983,可接受的线性范围为5.0-1000 ng / mL。因此,所有分析物的检出限≤1.0 ng / mL(S / N = 3),并且高富集因子在178.7-194.8范围内。此外,相应的重复性为4.0至8.7%(n = 3)。所提出的方法已成功地用于测定人体血清,废水和母乳样品中药物的痕量水平。将受体溶液转移到萃取池中,并在优化条件下再次进行SHS-HLLME程序。选择二丙胺(50 µL)作为萃取溶剂。引入的技术表现出良好的线性,测定素(R2)的系数高于0.983,可接受的线性范围为5.0-1000 ng / mL。因此,所有分析物的检出限≤1.0 ng / mL(S / N = 3),并且高富集因子在178.7-194.8范围内。此外,相应的重复性为4.0至8.7%(n = 3)。所提出的方法已成功地用于测定人体血清,废水和母乳样品中药物的痕量水平。将受体溶液转移到萃取池中,并在优化条件下再次进行SHS-HLLME程序。选择二丙胺(50 µL)作为萃取溶剂。引入的技术表现出良好的线性,测定素(R2)的系数高于0.983,可接受的线性范围为5.0-1000 ng / mL。因此,所有分析物的检出限为≤1.0 ng / mL(S / N = 3),并且高富集因子在178.7-194.8范围内。此外,相应的重复性为4.0至8.7%(n = 3)。所提出的方法已成功地用于测定人体血清,废水和母乳样品中药物的痕量水平。选择二丙胺(50 µL)作为萃取溶剂。引入的技术表现出良好的线性,测定素(R2)的系数高于0.983,可接受的线性范围为5.0-1000 ng / mL。因此,所有分析物的检出限≤1.0 ng / mL(S / N = 3),并且高富集因子在178.7-194.8范围内。此外,相应的重复性为4.0至8.7%(n = 3)。所提出的方法已成功用于测定人体血清,废水和母乳样品中药物的痕量水平。选择二丙胺(50 µL)作为萃取溶剂。引入的技术表现出良好的线性,测定素(R2)的系数高于0.983,可接受的线性范围为5.0-1000 ng / mL。因此,所有分析物的检出限≤1.0 ng / mL(S / N = 3),并且高富集因子在178.7-194.8范围内。此外,相应的重复性为4.0至8.7%(n = 3)。所提出的方法已成功地用于测定人体血清,废水和母乳样品中药物的痕量水平。所有分析物的浓度均为0 ng / mL(S / N = 3),并且高富集因子在178.7-194.8范围内。此外,相应的重复性为4.0至8.7%(n = 3)。所提出的方法已成功地用于测定人体血清,废水和母乳样品中药物的痕量水平。所有分析物的浓度均为0 ng / mL(S / N = 3),并且高富集因子在178.7-194.8范围内。此外,相应的重复性为4.0至8.7%(n = 3)。所提出的方法已成功地用于测定人体血清,废水和母乳样品中药物的痕量水平。
更新日期:2020-03-12
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