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采用分散固相萃取-活性炭球净化处理,结合气相色谱-质谱法测定鱼饲料中的双酚残留量。

Gas chromatography-mass spectrometric determination of bisphenol residues by dispersive solid phase extraction followed by activated carbon spheres cleanup from fish feed samples.

机构信息

Department of Chemistry, Acharya Nagarjuna University, Guntur, Andhra Pradesh, India.

Department of Chemistry, Government College for Women (A), Guntur, Andhra Pradesh, India.

出版信息

Eur J Mass Spectrom (Chichester). 2023 Jun;29(3):181-191. doi: 10.1177/14690667231174446. Epub 2023 May 15.

DOI:10.1177/14690667231174446
PMID:37186780
Abstract

Bisphenols are known endocrine disruptors commonly utilized in food packaging and storage materials, which frequently come into touch with multiple food products packed in them. The bisphenols in fish feed and other feed materials for aquatic organisms are harmful. The consumption of such marine foods is hazardous. Hence, the feed of aquatic products needs to be verified for the presence of bisphenols. The present study was focused on developing and validating a rapid, selective, and sensitive method to quantify 11 bisphenols from the fish feed with dispersive solid-phase extraction, which was cleaned by an optimized amount of activated carbon spheres and silylated by N,O-bis(trimethylsilyl)trifluoro acetamide and analyzed by gas chromatography-mass spectrometry. The new method was rigorously tested and verified after carefully tuning various parameters affecting analyte recovery. Limit of detection (LOD) were set at 0.5-5 ng/g and limit of quantification (LOQ) at 1-10 ng/g, respectively, resulting in 95-114% recoveries. Interday and intraday precisions in terms of relative standard deviation were found to be less than 11%. The proposed approach was effectively applied in floating and sinking fish feeds. The obtained results showed that higher concentration of bisphenol A, followed by bisphenol TMC, and bisphenol M at a concentration of 256.10, 159.01, and 168.82 ng/g in floating feed and 88.04, 200.79, and 98.03 ng/g in sinking feed samples, respectively.

摘要

双酚类物质是常见的内分泌干扰物,常用于食品包装和储存材料,这些材料经常与包装在其中的多种食品接触。鱼类饲料和其他水生生物饲料中的双酚类物质是有害的。食用这些海洋食品是有危险的。因此,需要对水产饲料进行双酚类物质的检测。本研究旨在开发和验证一种快速、选择性和灵敏的方法,用分散固相萃取法从鱼类饲料中定量分析 11 种双酚类物质,用优化量的活性炭球净化,并用 N,O-双(三甲基硅基)三氟乙酰胺硅烷化,并用气相色谱-质谱法分析。在仔细调整影响分析物回收率的各种参数后,对新方法进行了严格的测试和验证。检测限(LOD)设定在 0.5-5ng/g,定量限(LOQ)设定在 1-10ng/g,回收率为 95-114%。日内和日间精密度以相对标准偏差表示,均小于 11%。该方法有效地应用于漂浮和下沉的鱼饲料中。所得结果表明,在漂浮饲料中,双酚 A 的浓度最高,其次是双酚 TMC 和双酚 M,浓度分别为 256.10、159.01 和 168.82ng/g,在下沉饲料样品中,双酚 A 的浓度最高,其次是双酚 TMC 和双酚 M,浓度分别为 88.04、200.79 和 98.03ng/g。

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