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首页> 外文期刊>Journal of Agricultural and Food Chemistry >Gas Purge Microextraction Coupled with Stable Isotope Labeling-Liquid Chromatography/Mass Spectrometry for the Analysis of Bromophenols in Aquatic Products
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Gas Purge Microextraction Coupled with Stable Isotope Labeling-Liquid Chromatography/Mass Spectrometry for the Analysis of Bromophenols in Aquatic Products

机译:气体吹扫微萃取与稳定同位素标记-液相色谱/质谱联用分析水产品中的溴酚

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摘要

A green, sensitive, and accurate method was developed for the extraction and determination of bromophenols (BPs) from aquatic products by using organic solvent-free gas purge microsyringe extraction (GP-MSE) technique in combination with stable isotope labeling (SIL) strategy. BPs were extracted by NaHCO3 buffer solution, with recoveries varying from 92.0% to 98.5%. The extracted solution was analyzed by SIL strategy, during which analytes and standards were labeled by 10-methyl-acridone-2-sulfonyl chloride (d(0)-MASC) and its deuterated counterpart d(3)-MASC, respectively. The labeling reaction was finished within 10 min with good stability. The liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) sensitivity of BPs was greatly enhanced due to the mass-enhancing property of MASC, while the matrix effect was effectively minimized by the SIL strategy. The limits of detection (LODs) were in the range of 0.10-0.30 mu g/kg, while the limits of quantitations (LOQs) were in the range of 0.32-1.0 mu g/kg. The proposed method also showed great potential in the qualitative analysis of other bromophenols in the absence of standard.
机译:开发了一种绿色,灵敏,准确的方法,通过使用无溶剂有机气体吹扫微注射器萃取(GP-MSE)技术与稳定同位素标记(SIL)策略相结合,从水产品中萃取和测定溴酚(BP)。用NaHCO3缓冲溶液萃取BP,回收率从92.0%到98.5%不等。提取的溶液通过SIL策略进行分析,在此过程中,分析物和标准品分别用10-甲基-啶-2-磺酰氯(d(0)-MASC)和氘代的d(3)-MASC标记。标记反应在10分钟内以良好的稳定性完成。由于MASC的质量增强特性,大大提高了BP的液相色谱-串联质谱(HPLC-MS / MS)灵敏度,而SIL策略有效地降低了基质效应。检出限(LOD)在0.10-0.30μg / kg的范围内,而定量限(LOQ)在0.32-1.0μg / kg的范围内。所提出的方法在缺乏标准品的其他溴酚的定性分析中也显示出巨大的潜力。

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