{"title":"磁分散微固相萃取与中空纤维液相微萃取相结合预富集水样中的痕量毒死蜱农药","authors":"Reyhaneh Kouchakinejad, Shahab Shariati, Jafar Abolhasani, Ebrahim Ghorbani Kalhor, Mohammad Taghi Vardini, Ameneh Dorri","doi":"10.1007/s13738-024-03028-4","DOIUrl":null,"url":null,"abstract":"<div><p>In the present study, the integration of magnetic dispersive micro-solid-phase extraction (MD-µSPE) with hollow fiber liquid-phase microextraction (HF-LPME) prior to gas chromatography–mass spectrometry (GC/MS) was developed to preconcentrate and determine trace amounts of chlorpyrifos pesticide. <i>Azolla filiculoides</i> fern biomass was loaded by magnetite nanoparticles to prepare magnetic adsorbent (azolla@Fe<sub>3</sub>O<sub>4</sub>). The structural characteristics of the produced magnetic nanocomposites (MNCs) were investigated by FESEM, TEM, VSM, FTIR, EDX, and XRD methods. In the proposed MD-µSPE/HF-LPME method, the adsorption/desorption variables in MD-µSPE step were optimized by Taguchi fractional factorial design. After chlorpyrifos adsorption in the optimized condition of MD-µSPE (<i>V</i><sub>sample</sub> = 50 mL, contact time = 15 min, solution pH = 3, adsorbent mass = 0.05 g, ionic strength = 0.01 mol L<sup>−1</sup>, and eluent type = ethanol), 2.0 mL of the desorbed ethanolic solution was added to 16 mL of 10% (w/v) NaCl aqueous solution for the next HF-LPME method and the final analysis was performed by GC/MS. The developed method showed a limit of detection of 0.05 μg L<sup>−1</sup>, a limit of quantification of 0.5 μg L<sup>−1</sup>, a dynamic linear range of 0.5–1000.0 μg L<sup>−1</sup>, preconcentration factors between 700 and 1050, and a repeatability (RSD%) of 6.9%. The suitability of the MD-µSPE/HF-LPME method was confirmed by measuring chlorpyrifos in real samples with relative recoveries in the range of 97.0–108.5%. The results showed good accuracy and precision of the developed MD-µSPE/HF-LPME method for the preconcentration and determination of trace amounts of chlorpyrifos in the aqueous samples.</p><h3>Graphical abstract</h3>\n<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":676,"journal":{"name":"Journal of the Iranian Chemical Society","volume":null,"pages":null},"PeriodicalIF":2.2000,"publicationDate":"2024-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Magnetic dispersive micro-solid-phase extraction integrated with hollow fiber liquid-phase microextraction for preconcentration of trace amounts of chlorpyrifos pesticide in aqueous samples\",\"authors\":\"Reyhaneh Kouchakinejad, Shahab Shariati, Jafar Abolhasani, Ebrahim Ghorbani Kalhor, Mohammad Taghi Vardini, Ameneh Dorri\",\"doi\":\"10.1007/s13738-024-03028-4\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>In the present study, the integration of magnetic dispersive micro-solid-phase extraction (MD-µSPE) with hollow fiber liquid-phase microextraction (HF-LPME) prior to gas chromatography–mass spectrometry (GC/MS) was developed to preconcentrate and determine trace amounts of chlorpyrifos pesticide. <i>Azolla filiculoides</i> fern biomass was loaded by magnetite nanoparticles to prepare magnetic adsorbent (azolla@Fe<sub>3</sub>O<sub>4</sub>). The structural characteristics of the produced magnetic nanocomposites (MNCs) were investigated by FESEM, TEM, VSM, FTIR, EDX, and XRD methods. In the proposed MD-µSPE/HF-LPME method, the adsorption/desorption variables in MD-µSPE step were optimized by Taguchi fractional factorial design. After chlorpyrifos adsorption in the optimized condition of MD-µSPE (<i>V</i><sub>sample</sub> = 50 mL, contact time = 15 min, solution pH = 3, adsorbent mass = 0.05 g, ionic strength = 0.01 mol L<sup>−1</sup>, and eluent type = ethanol), 2.0 mL of the desorbed ethanolic solution was added to 16 mL of 10% (w/v) NaCl aqueous solution for the next HF-LPME method and the final analysis was performed by GC/MS. The developed method showed a limit of detection of 0.05 μg L<sup>−1</sup>, a limit of quantification of 0.5 μg L<sup>−1</sup>, a dynamic linear range of 0.5–1000.0 μg L<sup>−1</sup>, preconcentration factors between 700 and 1050, and a repeatability (RSD%) of 6.9%. The suitability of the MD-µSPE/HF-LPME method was confirmed by measuring chlorpyrifos in real samples with relative recoveries in the range of 97.0–108.5%. The results showed good accuracy and precision of the developed MD-µSPE/HF-LPME method for the preconcentration and determination of trace amounts of chlorpyrifos in the aqueous samples.</p><h3>Graphical abstract</h3>\\n<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>\",\"PeriodicalId\":676,\"journal\":{\"name\":\"Journal of the Iranian Chemical Society\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":2.2000,\"publicationDate\":\"2024-05-14\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of the Iranian Chemical Society\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://link.springer.com/article/10.1007/s13738-024-03028-4\",\"RegionNum\":4,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"CHEMISTRY, MULTIDISCIPLINARY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of the Iranian Chemical Society","FirstCategoryId":"92","ListUrlMain":"https://link.springer.com/article/10.1007/s13738-024-03028-4","RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"CHEMISTRY, MULTIDISCIPLINARY","Score":null,"Total":0}
Magnetic dispersive micro-solid-phase extraction integrated with hollow fiber liquid-phase microextraction for preconcentration of trace amounts of chlorpyrifos pesticide in aqueous samples
In the present study, the integration of magnetic dispersive micro-solid-phase extraction (MD-µSPE) with hollow fiber liquid-phase microextraction (HF-LPME) prior to gas chromatography–mass spectrometry (GC/MS) was developed to preconcentrate and determine trace amounts of chlorpyrifos pesticide. Azolla filiculoides fern biomass was loaded by magnetite nanoparticles to prepare magnetic adsorbent (azolla@Fe3O4). The structural characteristics of the produced magnetic nanocomposites (MNCs) were investigated by FESEM, TEM, VSM, FTIR, EDX, and XRD methods. In the proposed MD-µSPE/HF-LPME method, the adsorption/desorption variables in MD-µSPE step were optimized by Taguchi fractional factorial design. After chlorpyrifos adsorption in the optimized condition of MD-µSPE (Vsample = 50 mL, contact time = 15 min, solution pH = 3, adsorbent mass = 0.05 g, ionic strength = 0.01 mol L−1, and eluent type = ethanol), 2.0 mL of the desorbed ethanolic solution was added to 16 mL of 10% (w/v) NaCl aqueous solution for the next HF-LPME method and the final analysis was performed by GC/MS. The developed method showed a limit of detection of 0.05 μg L−1, a limit of quantification of 0.5 μg L−1, a dynamic linear range of 0.5–1000.0 μg L−1, preconcentration factors between 700 and 1050, and a repeatability (RSD%) of 6.9%. The suitability of the MD-µSPE/HF-LPME method was confirmed by measuring chlorpyrifos in real samples with relative recoveries in the range of 97.0–108.5%. The results showed good accuracy and precision of the developed MD-µSPE/HF-LPME method for the preconcentration and determination of trace amounts of chlorpyrifos in the aqueous samples.
期刊介绍:
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