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首页> 外文期刊>Analytica chimica acta >Comparative study of the instrumental couplings of high performance liquid chromatography with microwave-assisted digestion hydride generation atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry for chiral speciation of
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Comparative study of the instrumental couplings of high performance liquid chromatography with microwave-assisted digestion hydride generation atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry for chiral speciation of

机译:高效液相色谱仪与微波辅助消解氢化物发生原子荧光光谱法和电感耦合等离子体质谱法联用对手性物种的仪器比较研究

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摘要

A comparison of chiral separation and analysis of selenomethionine in breast and formula milk,using high performance liquid chromatography (HPLC) on a glycopeptide teicoplanin-based chiral stationary phase (Chirobiotic T),coupled to atomic fluorescence spectrometry (AFS) and inductively coupled plasma (ICP) MS detectors has been performed.The coupling HPLC-microwave-assisted digestion hydride generation requires on-line post-column analytes treatment,and a severe sample clean-up for fat and proteins elimination using centrifugation and ultrafiltration.Underivatized DL-selenomethionine enantiomers were completely resolved in 10 min using unbuffered water mobile phase at 1 ml min~(-1) flow.Good selectivity and sensitivities (detection limits 3.1 and 3.5 ng ml~(01)' as Se for L- and D-selenomethionine,respectively) were obtained,and method robustness and simplicity,together to the low cost of AFS detector,makes it suitable for infant milk routine analysis.HPLC-ICP-MS coupling exhibits very low detection limits (0.9 ng ml~(-1),as Se) for each DL-selenomethionine enantiomers,but the method suffers from matrix influence,that produces a poor S/N ratio and low reliability.The methods were applied to breast and formula milk samples with recoveries of 80% of the total selenium presence,which is attributable to the existence of other unknown species.L-Selenomethionine was the only isomer present in breast milk,but a 30% of D-selenomethionine was also detected in formula milk.
机译:使用基于肽肽替考拉宁的手性固定相(Chirobiotic T),高效液相色谱(HPLC),原子荧光光谱法(AFS)和电感耦合等离子体(HPLC)在乳房和配方奶中进行手性分离和硒代蛋氨酸分析的比较ICP)MS检测器已经完成,高效液相色谱-微波辅助消解氢化物的生成需要对柱后分析物进行在线处理,并且需要通过离心和超滤对脂肪和蛋白质进行彻底的样品净化。在非缓冲水流动相中以1 ml min〜(-1)流速在10分钟内完全分离。良好的选择性和灵敏性(检测限分别为L和D-硒代蛋氨酸的检测限3.1和3.5 ng ml〜(01)'作为Se) ),并且方法的鲁棒性和简便性,再加上AFS检测器的低成本,使其适用于婴儿牛奶常规分析.HPLC-ICP-MS耦合显示每种DL-硒代蛋氨酸对映体的检出限低(0.9 ng ml〜(-1),如Se),但该方法受基质影响,信噪比低,可靠性低。牛奶中存在的唯一异构体是L-硒代蛋氨酸,但在牛奶中也检出了30%的D-硒代蛋氨酸。配方奶。

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