{"title":"mil -101-海藻酸盐复合生物膜的合成及其在果蔬样品中磷沙酮微提取中的应用","authors":"Samira Aghaei Koltappeh , Zahra Ayazi","doi":"10.1016/j.foodchem.2025.145523","DOIUrl":null,"url":null,"abstract":"<div><div>A novel thin film microextraction (TFME) method was developed for phosalone determination in fruit and vegetable samples using gas chromatography-flame ionization detection (GC-FID). MIL-101 metal-organic framework (MOF) was synthesized via solvothermal condensation and incorporated into alginate (Alg) through solvent blending, forming a monolithic self-supportive thin film. The MIL-101/Alg biocomposite was characterized using XRD, FT-IR, and SEM. The impact of MIL-101 doping on extraction efficiency was assessed, showing significant enhancement. A central composite design (CCD) optimized extraction and desorption conditions. The method exhibited a detection limit of 1.6 ng mL<sup>−1</sup> and a quantification limit of 5.5 ng mL<sup>−1</sup>, with a linear range of 5.5–1000 ng mL<sup>−1</sup> (r<sup>2</sup> = 0.9909). Intra-day, inter-day, and inter-sorbent precisions (<em>n</em> = 6) were 3.6, 4.07, and 9.4 %, respectively. Validation in spiked real samples (apple, celery, cucumber, and tomato) showed relative recoveries above 93.2 %, confirming method accuracy and applicability.</div></div>","PeriodicalId":318,"journal":{"name":"Food Chemistry","volume":"492 ","pages":"Article 145523"},"PeriodicalIF":9.8000,"publicationDate":"2025-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Synthesis of MIL-101-alginate biocomposite as a novel self-supportive thin film for microextraction of phosalone in fruit and vegetable samples\",\"authors\":\"Samira Aghaei Koltappeh , Zahra Ayazi\",\"doi\":\"10.1016/j.foodchem.2025.145523\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>A novel thin film microextraction (TFME) method was developed for phosalone determination in fruit and vegetable samples using gas chromatography-flame ionization detection (GC-FID). MIL-101 metal-organic framework (MOF) was synthesized via solvothermal condensation and incorporated into alginate (Alg) through solvent blending, forming a monolithic self-supportive thin film. The MIL-101/Alg biocomposite was characterized using XRD, FT-IR, and SEM. The impact of MIL-101 doping on extraction efficiency was assessed, showing significant enhancement. A central composite design (CCD) optimized extraction and desorption conditions. The method exhibited a detection limit of 1.6 ng mL<sup>−1</sup> and a quantification limit of 5.5 ng mL<sup>−1</sup>, with a linear range of 5.5–1000 ng mL<sup>−1</sup> (r<sup>2</sup> = 0.9909). Intra-day, inter-day, and inter-sorbent precisions (<em>n</em> = 6) were 3.6, 4.07, and 9.4 %, respectively. Validation in spiked real samples (apple, celery, cucumber, and tomato) showed relative recoveries above 93.2 %, confirming method accuracy and applicability.</div></div>\",\"PeriodicalId\":318,\"journal\":{\"name\":\"Food Chemistry\",\"volume\":\"492 \",\"pages\":\"Article 145523\"},\"PeriodicalIF\":9.8000,\"publicationDate\":\"2025-07-14\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Food Chemistry\",\"FirstCategoryId\":\"97\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0308814625027748\",\"RegionNum\":1,\"RegionCategory\":\"农林科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"CHEMISTRY, APPLIED\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Food Chemistry","FirstCategoryId":"97","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0308814625027748","RegionNum":1,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"CHEMISTRY, APPLIED","Score":null,"Total":0}
引用次数: 0
摘要
建立了气相色谱-火焰离子化检测(GC-FID) -薄膜微萃取(TFME)法测定果蔬样品中磷沙酮的方法。采用溶剂热缩合法合成MIL-101金属有机骨架(MOF),并通过溶剂共混掺入海藻酸盐(Alg)中,形成整体自支撑薄膜。采用XRD、FT-IR和SEM对MIL-101/Alg生物复合材料进行了表征。研究了MIL-101对提取效率的影响,结果表明MIL-101对提取效率有显著提高。采用中心复合设计优化了萃取和解吸条件。方法检出限为1.6 ng mL−1,定量限为5.5 ng mL−1,线性范围为5.5 ~ 1000 ng mL−1 (r2 = 0.9909)。日内、日内、吸附间精密度(n = 6)分别为3.6、4.07、9.4 %。在添加的真实样品(苹果、芹菜、黄瓜和番茄)中验证,相对回收率高于93.2 %,证实了方法的准确性和适用性。
Synthesis of MIL-101-alginate biocomposite as a novel self-supportive thin film for microextraction of phosalone in fruit and vegetable samples
A novel thin film microextraction (TFME) method was developed for phosalone determination in fruit and vegetable samples using gas chromatography-flame ionization detection (GC-FID). MIL-101 metal-organic framework (MOF) was synthesized via solvothermal condensation and incorporated into alginate (Alg) through solvent blending, forming a monolithic self-supportive thin film. The MIL-101/Alg biocomposite was characterized using XRD, FT-IR, and SEM. The impact of MIL-101 doping on extraction efficiency was assessed, showing significant enhancement. A central composite design (CCD) optimized extraction and desorption conditions. The method exhibited a detection limit of 1.6 ng mL−1 and a quantification limit of 5.5 ng mL−1, with a linear range of 5.5–1000 ng mL−1 (r2 = 0.9909). Intra-day, inter-day, and inter-sorbent precisions (n = 6) were 3.6, 4.07, and 9.4 %, respectively. Validation in spiked real samples (apple, celery, cucumber, and tomato) showed relative recoveries above 93.2 %, confirming method accuracy and applicability.
期刊介绍:
Food Chemistry publishes original research papers dealing with the advancement of the chemistry and biochemistry of foods or the analytical methods/ approach used. All papers should focus on the novelty of the research carried out.